CN110328916B - Preparation method of flame-retardant and electromagnetic shielding sandwich heat-insulating material - Google Patents
Preparation method of flame-retardant and electromagnetic shielding sandwich heat-insulating material Download PDFInfo
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Abstract
The invention discloses a preparation method of a flame-retardant and electromagnetic shielding sandwich thermal insulation material, which is characterized in that a novel electromagnetic shielding and flame-retardant composite non-woven fabric is prepared at a proper reaction temperature and time by adopting a certain content of adhesive, carbon fiber cloth and aromatic sulfone polyamide cloth, then the composite non-woven fabric is compounded with rigid polyurethane foam through a 'two-step method', and the structure of the polyurethane thermal insulation material is designed to prepare the novel sandwich thermal insulation material with excellent flame retardance and electromagnetic shielding performance, so that the processing technology is simplified, the cost is reduced, and the novel sandwich thermal insulation material has important economic benefit and social benefit.
Description
Technical Field
The invention relates to the technical field of preparation of composite materials, in particular to a preparation method of a flame-retardant and electromagnetic shielding sandwich heat-insulating material.
Background
Flame retardancy refers to the property of a substance or material that, after treatment, has a significant delay in the spread of a flame. With the increase of safety awareness, the demand for flame retardancy has been increasing for materials used in construction materials, vehicles, home appliances, and the like. There are many methods for evaluating flame retardancy, such as oxygen index measurement, horizontal or vertical burning test, and the like. In the last 10 years, 3.1 thousands of high-rise building fires occur all over the country, 474 people die, and the direct property loss is 15.6 million yuan. Since the heat-insulating outer wall of a building and furniture are highly flammable materials, the fire can be completely burnt after being ignited for 5 to 10 minutes. Currently, combustible materials are generally endowed with certain flame retardant properties by adding flame retardants and modifying raw materials, and commonly used flame retardants include halogen-based flame retardants and inorganic flame retardants. The halogen flame retardant is the flame retardant with the largest output all over the world at present, mainly represented by chlorine flame retardant and bromine flame retardant, and is widely applied to various fields for a long time due to high flame retardant efficiency and low price. Although the halogen flame retardant has good flame retardant effect and large market demand, a large amount of smoke, corrosive and toxic gas harmful to human bodies and the environment is generated when the halogen flame retardant is combusted. The inorganic additive flame retardant has the advantages of low price, low toxicity, durable flame retardant effect, difficult volatilization and precipitation, small smoke yield and the like, but the problems of excessive addition, large granularity and the like can influence the mechanical property of the material and the forming process of the polymer. And the defects are more prominent, the flame retardant efficiency is poor, the flame retardant requirement can be met only by larger filling amount, and the influence on the mechanical and mechanical properties of the base material is larger. The phosphorus flame retardant can act in a gas phase and can also act in a condensed phase, and toxic gas is not generated in the combustion process. Therefore, phosphorus-based flame retardants have been drawing attention.
With the rapid development of scientific technology, the proliferation of various electronic devices in industrial and domestic environments has caused a great deal of electromagnetic interference. Electromagnetic radiation has seriously affected people's lives and has become another serious pollution-electromagnetic pollution-which can be compared with water pollution and air pollution in modern life. At the same time, the problem of electromagnetic shielding has affected almost all electrical and electronic systems, from daily life to military activities to space exploration. Taking a notebook computer as an example, the power system of the notebook computer can generate electromagnetic radiation energy with a wide frequency band, and the radiated energy can be transmitted and picked up by a television antenna, a wireless remote controller and any other equipment to cause performance abnormity. In addition, the long-term exposure of a living body to electromagnetic energy often increases the risk of various diseases, such as subjective neurological symptoms, cardiovascular disorders, reproductive dysfunction, and various systemic cancers. Also, the use of mobile phones and the like is not allowed during flight or in intensive care units of hospitals due to the presence of electromagnetic radiation. Therefore, the solution to the problems of electromagnetic radiation and electromagnetic interference is not very slow.
The polysulfonamide PSA fiber for short consists of polysulfonamide, is a novel high-technology fiber product independently developed in China, and has excellent heat resistance, flame retardance and filtering performance, excellent physical and mechanical properties and excellent chemical stability. The long-term service temperature of the polysulfonamide fibers is 250 ℃, the strength retention rate is more than 80 percent after 100h heating, and the Limiting Oxygen Index (LOI) is 33 percent. Polysulfonamide is widely applied to the fields of protective products, building materials, aerospace, national defense war industry and the like, and is mixed with other fibers for use to make up for the defects of other fibers.
The carbon fiber has good electromagnetic shielding performance and is a high-performance reinforced fiber. Meanwhile, the carbon fiber has excellent electric and thermal conductivity, good flame retardant property, extremely low thermal expansion coefficient, low radiation ray absorption, non-magnetism, no magnetization, excellent vibration damping property, fatigue resistance and creep resistance. The main reason for the electromagnetic shielding capability of carbon fiber is that it has good electrical conductivity. The volume resistivity of the carbon fiber is usually between (0.8-1.8) multiplied by 10-3 omega cm, and the electric conductivity is increased along with the increase of the heat treatment temperature. Therefore, the carbon fiber can be an excellent reflection material of electromagnetic waves after being subjected to high-temperature graphitization treatment. At present, domestic research on carbon fibers mainly focuses on the mechanical properties of composite materials, and research in the field of electromagnetic shielding is relatively rare.
The existing flame-retardant electromagnetic shielding non-woven fabric is processed into flame-retardant and electromagnetic shielding non-woven fabric mainly by the processes of spinning, weaving, sizing and the like. But the process is complex and the cost is high, which can not meet the production requirement.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, a method for preparing a flame-retardant and electromagnetic shielding sandwich thermal insulation material is provided, a novel electromagnetic shielding and flame-retardant composite non-woven fabric is prepared at a proper reaction temperature and time by adopting a certain content of waterborne polyurethane, carbon fiber cloth and aromatic sulfone polyester cloth, then the composite non-woven fabric is compounded with rigid polyurethane foam through a two-step method, and the structure of the polyurethane thermal insulation material is designed to prepare the novel sandwich thermal insulation material with excellent flame retardance and electromagnetic shielding performance, so that the processing process is shortened, the production cost is reduced, and the method has important economic benefits and social benefits.
The preparation method of the flame-retardant and electromagnetic shielding sandwich thermal insulation material comprises composite non-woven fabrics and rigid polyurethane foam, wherein the composite non-woven fabrics are provided with an upper layer, a middle layer and a lower layer, the rigid polyurethane foam is filled between every two composite non-woven fabrics, and the composite non-woven fabrics are formed by compounding carbon fiber fabrics, adhesives and aromatic sulfone polyester fabrics.
As a further improvement of the above aspect, the adhesive is provided as a water-based polyurethane.
As a further improvement of the scheme, the method comprises the following steps:
the method comprises the following steps: uniformly coating an adhesive on carbon fiber cloth and polysulfonamide cloth, compounding the carbon fiber cloth and the polysulfonamide cloth, drying, and drying in a constant-temperature and constant-humidity environment to prepare the composite non-woven fabric;
step two: uniformly stirring polyether polyol and a phosphorus flame retardant, adding isocyanate, stirring for the second time to prepare the rigid polyurethane foam, quickly injecting the rigid polyurethane foam into a mold with the upper layer and the lower layer both paved with the composite non-woven fabric, integrally molding, curing, and demolding to obtain a preformed product;
step three: and (2) uniformly stirring polyether polyol and a phosphorus flame retardant, adding isocyanate, stirring for the second time to prepare the rigid polyurethane foam, injecting the rigid polyurethane foam into a mold with the upper layer paved with the composite non-woven fabric and the lower layer paved with the preformed product, integrally molding, curing, and demolding to obtain the sandwich heat-insulating material with flame retardance and electromagnetic shielding performance.
As a further improvement of the above scheme, in the second step, the mass ratio of the polyether polyol, the phosphorus flame retardant and the isocyanate is 5: 1: 5.
as a further improvement of the above scheme, in the second step and the third step, the stirring speed of the polyether polyol and the phosphorus flame retardant is 1200rpm/min, and the stirring time is 15 min; the rotating speed of adding the isocyanate for secondary stirring is 1200rpm/min, and the stirring time is 12-16 s.
As a further improvement of the above scheme, the preparation of the composite non-woven fabric in the first step specifically comprises: the adhesive is uniformly coated on carbon fiber cloth and polysulfonamide cloth through a high-pressure liquid gun, the carbon fiber cloth and the polysulfonamide cloth are compounded together, dried in an environment with the temperature of 80-100 ℃, and then dried in a constant-temperature and constant-humidity environment with the temperature of 25 ℃ and the humidity of 53 percent to prepare the aromatic polyamide fiber cloth.
As a further improvement of the scheme, in the first step, the drying temperature is 90 ℃, and the drying time is 10-15 minutes.
As a further improvement of the above aspect, in the second step, the phosphorus-based flame retardant is set to be a phosphate flame retardant.
As a further improvement of the above scheme, in the second step, the curing time is set to 1 h.
As a further improvement of the above scheme, in the second step and the third step, the length, width and height of the die are sequentially set to 350mm, 330mm and 10 mm; the length and the width of the composite non-woven fabric prepared in the step one are 350mm and 330 mm; the length, width and height of the preformed product prepared in the step two are 350mm, 330mm and 10mm in sequence; the length, the width and the height of the sandwich thermal insulation material prepared in the third step are 350mm, 330mm and 20mm in sequence, 25g of the adhesive is set in the first step, and the use amounts of the polyether polyol, the phosphorus flame retardant and the isocyanate in the second step are 90g, 18g and 90g respectively.
The invention has the beneficial effects that:
compared with the prior art, the preparation method of the flame-retardant and electromagnetic shielding sandwich thermal insulation material provided by the invention has the advantages that a novel electromagnetic shielding and flame-retardant composite non-woven fabric is prepared at a proper reaction temperature and time by adopting a certain content of adhesive, carbon fiber cloth and aromatic sulfone polyamide cloth, then the composite non-woven fabric is compounded with rigid polyurethane foam through a two-step method, and the novel sandwich thermal insulation material with excellent flame retardance and electromagnetic shielding performance is prepared by designing the structure of the polyurethane thermal insulation material, so that the processing technology is simplified, the cost is reduced, and the preparation method has important economic benefits and social benefits.
Drawings
The following detailed description of embodiments of the invention is provided in conjunction with the appended drawings, in which:
FIG. 1 is a schematic structural view of a sandwich insulation material of the present invention;
FIG. 2 is a representation of the flame retardant and electromagnetic shielding properties of the sandwich insulation material of the present invention.
Detailed Description
As shown in figure 1, the novel flame-retardant and electromagnetic shielding sandwich thermal insulation material provided by the invention comprises composite non-woven fabrics and rigid polyurethane foam, wherein the composite non-woven fabrics are provided with an upper layer, a middle layer and a lower layer, the rigid polyurethane foam is filled between every two composite non-woven fabrics, and the composite non-woven fabrics are formed by compounding carbon fiber fabrics, adhesives and aromatic sulfone polyester fabrics. Specifically, the adhesive is set to be water-based polyurethane.
The preparation method comprises the following steps: the method comprises the following steps: uniformly coating an adhesive on the carbon fiber cloth and the polysulfonamide cloth, compounding the carbon fiber cloth and the polysulfonamide cloth, drying, and drying in a constant-temperature and constant-humidity environment to prepare a composite non-woven fabric; step two: uniformly stirring polyether polyol and a phosphorus flame retardant, adding isocyanate, and stirring for the second time to prepare rigid polyurethane foam, (wherein the phosphorus flame retardant is a phosphate flame retardant), quickly injecting the rigid polyurethane foam into a mold with an upper layer and a lower layer both paved with composite non-woven fabrics, integrally molding, curing, and demolding to obtain a preformed product; step three: and (3) preparing the rigid polyurethane foam in the step two, injecting the rigid polyurethane foam into a mold with the upper layer paved with the composite non-woven fabric and the lower layer paved with the preformed product to be integrally formed, and demolding after curing for 1h to obtain the sandwich heat-insulating material with flame retardance and electromagnetic shielding performance.
The preparation of the composite non-woven fabric in the first step specifically comprises the following steps: the adhesive, namely the waterborne polyurethane, is uniformly coated on the carbon fiber cloth and the polysulfonamide cloth through a high-pressure liquid gun, the carbon fiber cloth and the polysulfonamide cloth are compounded together, dried at the temperature of 80-100 ℃, and then dried at the constant temperature and humidity of 25 ℃ to prepare the waterborne polyurethane adhesive. When the test was carried out at 70 ℃, 90 ℃ and 110 ℃ for 10min, the adhesion at 70 ℃ was found to be poor; aging the waterborne polyurethane at 110 ℃; therefore, the temperature is selected to be 90 ℃, and then the reaction is carried out for 5min, 10min and 15min at different drying times at 90 ℃, and the good adhesion can be achieved after 10min, so that the reaction time is 10 min.
In the second step and the third step, the mass ratio of the polyether polyol, the phosphorus flame retardant and the isocyanate is 5: 1: 5, in the second step and the third step, the stirring speed of the polyether polyol and the phosphorus flame retardant is 1200rpm/min, and the stirring time is 15 min; the rotating speed of adding isocyanate for secondary stirring is 1200rpm/min, and the stirring time is 12-16 s. In practical application, the length, width and height of the die can be set to 350mm, 330mm and 10mm in sequence; correspondingly, the length and the width of the composite non-woven fabric prepared in the step one are 350mm and 330 mm; the length, width and height of the preformed product prepared in the step two are 350mm, 330mm and 10mm in sequence; the length, width and height of the sandwich thermal insulation material prepared in the third step are 350mm, 330mm and 20mm in sequence, correspondingly, the adhesive, namely the waterborne polyurethane is set to be 25g in the first step, and tests (15g, 20g, 25g and 30g) prove that the 25g of the waterborne polyurethane can be coated with the carbon fiber cloth and the polysulfonamide cloth which are 350mm multiplied by 330mm, and the thickness of the waterborne polyurethane is about 20um at the moment. Correspondingly, the preparation of the rigid polyurethane foam in the step two specifically comprises the following steps: 90g of polyether polyol and 18g of phosphorus flame retardant are taken, stirred for 15min at 1200rpm/min by using a direct current servo electric stirrer, and then 90g of isocyanate is added and stirred for 12s-16s at 1200 rpm/min. Wherein the model of the DC servo electric stirrer is set to be S569T 2/A3. Tests show that the limit oxygen index of the sandwich thermal insulation material prepared by the invention is 27%, and the electromagnetic shielding value can reach 40dB, and is shown in figure 2.
The above embodiments are not limited to the technical solutions of the embodiments themselves, and the embodiments may be combined with each other into a new embodiment. The above embodiments are only for illustrating the technical solutions of the present invention and are not limited thereto, and any modification or equivalent replacement without departing from the spirit and scope of the present invention should be covered within the technical solutions of the present invention.
Claims (6)
1. A preparation method of a flame-retardant and electromagnetic shielding sandwich thermal insulation material is characterized by comprising the following steps: the sandwich thermal insulation material comprises composite non-woven fabrics and rigid polyurethane foam, wherein the composite non-woven fabrics are provided with an upper layer, a middle layer and a lower layer, the rigid polyurethane foam is filled between every two composite non-woven fabrics, the composite non-woven fabrics are formed by compounding carbon fiber fabrics, adhesive and polysulfonamide fabrics, the adhesive is aqueous polyurethane, and the preparation method comprises the following steps:
the method comprises the following steps: uniformly coating an adhesive on carbon fiber cloth and polysulfonamide cloth, compounding the carbon fiber cloth and the polysulfonamide cloth, drying, and drying in a constant-temperature and constant-humidity environment to prepare the composite non-woven fabric, wherein the length and the width of the composite non-woven fabric prepared in the first step are 350mm and 330mm, and the amount of the adhesive in the first step is 25 g;
step two: uniformly stirring polyether polyol and a phosphorus flame retardant, adding isocyanate, stirring for the second time to prepare rigid polyurethane foam, quickly injecting the rigid polyurethane foam into a mold with an upper layer and a lower layer both paved with the composite non-woven fabric, integrally molding, curing, and demolding to obtain a preform, wherein the use amounts of the polyether polyol, the phosphorus flame retardant and the isocyanate in the second step are 90g, 18g and 90g respectively;
step three: and (2) uniformly stirring polyether polyol and a phosphorus flame retardant, adding isocyanate, stirring for the second time to prepare the rigid polyurethane foam, injecting the rigid polyurethane foam into a mold with the upper layer paved with the composite non-woven fabric and the lower layer paved with the preformed product, integrally molding, curing, and demolding to obtain the sandwich heat-insulating material with flame retardance and electromagnetic shielding performance.
2. The method for preparing the flame-retardant and electromagnetic shielding sandwich thermal insulation material according to claim 1, which is characterized in that: in the second step and the third step, the stirring speed of the polyether polyol and the phosphorus flame retardant is 1200rpm/min, and the stirring time is 15 min; the rotating speed of adding the isocyanate for secondary stirring is 1200rpm/min, and the stirring time is 12-16 s.
3. The method for preparing the flame-retardant and electromagnetic shielding sandwich thermal insulation material according to claim 1, which is characterized in that: the preparation of the composite non-woven fabric in the first step specifically comprises the following steps: the adhesive is uniformly coated on carbon fiber cloth and polysulfonamide cloth through a high-pressure liquid gun, the carbon fiber cloth and the polysulfonamide cloth are compounded together, dried in an environment with the temperature of 80-100 ℃, and then dried in a constant-temperature and constant-humidity environment with the temperature of 25 ℃ and the humidity of 53 percent to prepare the aromatic polyamide fiber cloth.
4. The method for preparing the flame-retardant and electromagnetic shielding sandwich thermal insulation material according to claim 3, characterized in that: in the first step, the drying temperature is 90 ℃, and the drying time is 10-15 minutes.
5. The method for preparing the flame-retardant and electromagnetic shielding sandwich thermal insulation material according to claim 1, which is characterized in that: and in the second step, the phosphorus flame retardant is set to be a phosphate flame retardant.
6. The method for preparing the flame-retardant and electromagnetic shielding sandwich thermal insulation material according to claim 5, characterized in that: in the second step, the curing time is set to 1 h.
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