Fireproof insulating material and preparation method thereof

Abstract

The invention discloses a fireproof insulating material and a preparation method thereof, and the fireproof insulating material comprises the following raw materials in percentage by weight: 20-30% of silicon resin, 20-30% of phenolic modified epoxy resin, 7.5-10% of an epoxy curing agent, 5-6% of an isophorone diisocyanate curing agent, 0.5-1% of a flatting agent, 0.2-0.5% of an electricity increasing agent type powdering aid, 0.3-0.5% of benzoin, 0.3-0.5% of an antioxidant and the balance of a solvent. 11.3-15% of a flame-retardant and fire-resistant functional auxiliary agent, and the balance of a pigment and a filler; the filler is a composition prepared from glass powder, mica powder, aluminum phosphate and wollastonite in a mass ratio of (8-10): (4-5): (2.6-3): (4-4.5). Through the mode, when the fireproof insulating material is used, the surface of a protected workpiece is coated with the powder, a protective coating is formed after baking and curing, and the curing conditions are 230 DEG C and 30 min; the protective coating has good initial insulation performance, still has good insulation effect after being burned in open fire at 1300 DEG C for 30 min, and can pass insulation performance tests after the initial coating and open fire burning: alternating voltage AC is 3000V, test duration is 60s, and current is less than 1mA.

Description

Technical Field

[0001] The present invention relates to the technical field of fireproof insulation, and particularly relates to a fireproof insulation material and a preparation method thereof. Background Art

[0002] Organic-inorganic composite insulation materials are new insulation materials composed of organic materials and inorganic materials. Organic materials usually have good flexibility and processing performance, while inorganic materials have good heat resistance and strong corrosion resistance. After combining the two, materials with excellent performance can be obtained. Due to these excellent properties, it can be used in the electrical insulation field to manufacture insulation layers of electrical equipment such as cables, transformers, and motors, in electronic packaging to manufacture packaging materials for electronic devices such as integrated circuits and semiconductor devices, in the aerospace field to manufacture structural materials and insulation materials for aircraft, rockets and other aerospace vehicles, and also has extensive applications in the fields of automobiles, buildings, etc.

[0003] For example, the patent of Chinese Patent CN 222097208U discloses a fireproof mica tape for battery packs. This mica tape is made by double compound pressing of epoxy resin and fiberglass cloth. The preparation cycle of this process is long and the equipment turnover is slow. The patent of Chinese Patent CN221460285U discloses a composite fiberglass thermal insulation and flame retardant diaphragm, which has a fiberglass thermal insulation and flame retardant material sealed between a PET modified film and a ceramic heat insulation film to achieve the effects of heat insulation and flame retardancy. However, the above-mentioned fireproof insulation materials have fixed shapes and can only be used as surface coating materials, and there are construction problems for the painting protection of special-shaped parts, and their temperature resistance and pressure resistance far cannot meet the new functions and performance requirements of new energy and electric vehicles.

[0004] For another example, the bond energy of Si-O is higher than that of C-O. Some high-temperature resistant insulation materials improve the temperature resistance of the coating by adding silicone resin, and at the same time add epoxy resin to enhance the insulation effect of the coating. However, the temperature resistance of such organic coatings cannot reach 800 °C. Summary of the Invention

[0005] Aiming at the above-mentioned shortcomings of the prior art, the present invention provides a fireproof insulation material and a preparation method thereof.

[0006] To achieve the above objectives, the present invention is realized through the following technical solutions: A fireproof insulation material, characterized in that it comprises raw materials in the following weight percentages: silicone resin 20-30%, phenolic modified epoxy resin 20-30%, epoxy curing agent 7.5-10%, isophorone diisocyanate curing agent: 5-6%, leveling agent 0.5-1%, electrification agent type powdering aid 0.2-0.5%, benzoin 0.3-0.5%, antioxidant 0.3-0.5%, flame retardant and fire-resistant functional aid 11.3-15%, and the balance is pigments and fillers.

[0007] As a preferred embodiment, the filler is a composition prepared from glass powder, mica powder, aluminum phosphate, and wollastonite according to a mass ratio of (8 - 10) : (4 - 5) : (2.6 - 3) : (4 - 4.5), and all are commercially available products.

[0008] As a preferred embodiment, the silicone resin is a pure phenyl silicone resin with 100% organosilicon content and a hydroxyl content of 2.5 - 7 wt%. For example, the silicone resin AH061 of Aohan Protection Technology or WACKER SILRES® 604. Selecting a silicone resin in the film-forming substance can provide the initial high-temperature resistance of the coating film, and the hydroxyl groups contained in both resins can crosslink and cure with the isophorone diisocyanate curing agent, improving the crosslinking density of the entire coating film, so that the coating film has good chemical resistance and initial mechanical properties.

[0009] As a preferred embodiment, the epoxy equivalent of the phenolic-modified epoxy resin is 750 - 900 g / eq, and the viscosity is 1000 - 4000 cps / 150 °C. For example, Araldite GT 7255 of HUNTSMAN or KD211S of Guodu Chemical. The phenolic-modified epoxy resin crosslinks and cures with the phenolic curing agent, providing the initial electrical insulation performance and excellent mechanical properties for the coating film.

[0010] As a preferred embodiment, the epoxy curing agent is a resin capped with phenolic hydroxyl groups, with a hydroxyl value of 230 - 260 mgKOH / g and a softening point of 80 - 100 °C. For example, V-2051W of Shaanxi Jinchen Yongyue New Materials or KD405 of Guodu Chemical, which can crosslink and cure with the phenolic-modified epoxy resin or bisphenol A epoxy resin to maintain the coating performance.

[0011] As a preferred embodiment, the isophorone diisocyanate curing agent has an NCO value of 14 - 16 mgKOH / g and a glass transition temperature Tg of 45 - 55 °C. For example, VETAGON ® B1530 of Evonik, Crelan ® NW-5 of Covestro, Jietongda K7150, etc. During the curing process, it reacts with the hydroxyl groups of the silicone resin to improve the performance of the coating.

[0012] As a preferred embodiment, the flame retardant and fire-resistant functional agent used is the commercially available DM95-G720B of Anmi Weina, which ensures that no open flame appears when the coating is ablated by an open flame at high temperature, achieving the effect of slow temperature rise, so that the coating can remain intact after ablation.

[0013] As a preferred embodiment, the leveling agent is an acrylate leveling agent. For example, ADDITOL® P896 of Allnex, which can promote the fluidity and compatibility between components, especially the compatibility between the silicone resin and epoxy resin systems, making the entire coating exhibit the best performance.

[0014] As a preferred solution, the electrostatic charging powdering aid is a quaternary ammonium salt powdering aid, such as PTN601 of Patna, which can improve the electrostatic charging effect of the powder coating product during the construction process, making the whole system have excellent construction effect and edge wrapping performance.

[0015] A preparation method of a fireproof and insulating material as described above, which comprises the following steps: S1. Premix silicone resin, phenolic modified epoxy resin, phenolic curing agent, isophorone diisocyanate curing agent, leveling agent, powdering aid, benzoin, antioxidant and flame retardant and fireproof functional aid into component A, and premix pigment and filler into component B; S2. After mixing component A and component B evenly, extrude at 100 - 110 °C to obtain a molten material; S3. After pressing the molten material into tablets, grind it into powder, and that's it.

[0016] As a preferred solution, in step S1, when premixing component A and component B, control the stirring speed at 100 - 300 rpm and the premixing time at 2 - 10 min. In step S2, when mixing component A and component B, control the stirring speed at 100 - 300 rpm and the mixing time at 2 - 10 min.

[0017] As a preferred solution, the extrusion process is carried out in a twin - screw extruder, and control the rotation speed of the twin - screw extruder at 1500 rpm.

[0018] In order to better achieve the purpose of the present invention, the present invention also provides a fireproof and insulating material prepared according to the described preparation method.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: When the fireproof and insulating material of the present invention is used, the powder is coated on the surface of the workpiece to be protected, and a protective coating is formed after baking and curing. The curing conditions are: 230 °C, 30 min; The protective coating not only has good original insulation performance, but also has good insulation effect after being exposed to an open fire at 1300 °C for 30 min. Both the initial coating and the coating after being ablated by an open fire can pass the insulation performance test: AC voltage 3000V, test duration 60 s, current < 1 mA. The present invention provides a fireproof and insulating material that can be spray - constructed, broadening the application scenarios of the product. Specific embodiments

[0020] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the scope of protection of the present invention.

[0021] I. Embodiment 1 A preparation method of a fireproof and insulating material is provided in this embodiment, which specifically includes the following steps: I. Weigh the raw materials according to the following mass fractions: Component A: Pure phenyl silicone resin AH061: 25 kg, phenolic modified epoxy resin Araldite GT 7255: 25 kg, epoxy curing agent KD405: 7.5 kg, isophorone diisocyanate curing agent VETAGON® B1530: 5 kg, acrylate leveling agent ADDITOL® P 896: 1 kg, PTN601: 0.5 kg, benzoin: 0.5 kg, antioxidant: 0.5 kg, fireproof and fire-resistant functional agent DM95-G720B: 14.6 kg.

[0022] Component B: Pigment 0.8 kg; glass powder: 8 kg; mica powder: 5 kg; aluminum phosphate: 2.6 kg; wollastonite: 4 kg.

[0023] II. Premix the raw materials of Component A and Component B separately, control the stirring speed during premixing at 100 - 300 rpm, and the premixing time at 2 - 10 min. Then mix Component A and Component B together, control the stirring speed during mixing at 100 rpm, and the mixing time at 5 - 10 min.

[0024] III. Rapidly extrude the mixed material through a twin-screw extruder, with the extrusion temperature at 100 - 110 °C and the extruder speed at 1500 rpm.

[0025] IV. Use a cold roll and a tablet press to press and cool the extruded molten material.

[0026] V. After cooling, put the material into a grinding equipment to grind it into powder, thus obtaining the fireproof and insulating material.

[0027] II. Embodiment 2 A preparation method of a fireproof and insulating material is provided in this embodiment, which specifically includes the following steps: I. Weigh the raw materials according to the following mass fractions: Component A: Pure phenyl silicone resin AH061: 20 kg, phenolic modified epoxy resin Araldite GT 7255: 30 kg, epoxy curing agent KD405: 10 kg, isophorone diisocyanate curing agent K7150: 5 kg, acrylate leveling agent ADDITOL® P 896: 0.5 kg, PTN601: 0.2 kg, benzoin: 0.3 kg, antioxidant: 0.2 kg, flame retardant and fire resistant functional agent DM95 - G720B: 11.3 kg.

[0028] Component B: Pigment 1 kg; Filler: Glass powder: 10 kg; Mica powder: 4 kg; Aluminum phosphate: 3 kg; Wollastonite: 4.5 kg.

[0029] II. Premix the raw materials of Component A and Component B separately, control the stirring speed during premixing at 100 - 300 rpm and the premixing time at 2 - 10 min, then mix Component A and Component B together, control the stirring speed during mixing at 100 rpm and the mixing time at 5 - 10 min.

[0030] III. Rapidly extrude the mixed material through a twin - screw extruder, the extrusion temperature is 100 - 110 °C, and the rotational speed of the extruder is 1500 rpm.

[0031] IV. Use a cold roll and a tablet press to cool and press the extruded molten material.

[0032] V. After cooling, put the material into a grinding equipment to grind it into powder, thus obtaining the fire - proof and insulating material.

[0033] III. Example 3 In this example, a preparation method of a fire - proof and insulating material is provided, which specifically includes the following steps: I. Weigh the raw materials according to the following mass fractions: Component A: Pure phenyl silicone resin AH061: 30 kg, phenolic modified epoxy resin KD211S: 20 kg, epoxy curing agent V - 2051W: 7.5 kg, isophorone diisocyanate curing agent Crelan ®NW - 5: 6 kg, acrylate leveling agent ADDITOL® P 896: 0.5 kg, PTN601: 0.4 kg, benzoin: 0.4 kg, antioxidant: 0.4 kg, flame retardant and fire resistant functional agent DM95 - G720B: 15 kg.

[0034] Component B: Pigment 0.8 kg; Filler: Glass powder: 8 kg; Mica powder: 4 kg; Aluminum phosphate: 3 kg; Wollastonite: 4 kg.

[0035] II. Premix the raw materials of component A and component B separately, control the stirring speed during premixing to be 100 - 300 rpm, and the premixing time to be 2 - 10 min. Then mix component A and component B together, control the stirring speed during mixing to be 100 rpm, and the mixing time to be 5 - 10 min.

[0036] III. Rapidly extrude the mixed material through a twin - screw extruder, with the extrusion temperature being 100 - 110 °C and the extruder speed being 1500 rpm.

[0037] IV. Use a cold roll and a tablet press to press and cool the extruded molten material.

[0038] V. After cooling, put the material into a grinding device to grind it into powder, thus obtaining the fire - proof insulating material.

[0039] IV. Example 4 In this example, a preparation method of a fire - proof insulating material is provided, which specifically includes the following steps: I. Weigh the raw materials according to the following mass fractions: Component A: Pure phenyl silicone resin SILRES® 604: 25 kg, phenolic - modified epoxy resin Araldite GT 7255: 25 kg, epoxy curing agent KD405: 7.5 kg, isophorone diisocyanate curing agent VETAGON ® B1530: 5 kg, acrylate - type leveling agent ADDITOL® P 896: 1 kg, PTN601: 0.5 kg, benzoin: 0.5 kg, antioxidant: 0.5 kg, fire - retardant and fire - resistant functional agent DM95 - G720B: 14.6 kg.

[0040] Component B: Pigment 0.8 kg; glass powder: 8 kg; mica powder: 5 kg; aluminum phosphate: 2.6 kg; wollastonite: 4 kg.

[0041] II. Premix the raw materials of component A and component B separately, control the stirring speed during premixing to be 100 - 300 rpm, and the premixing time to be 2 - 10 min. Then mix component A and component B together, control the stirring speed during mixing to be 100 rpm, and the mixing time to be 5 - 10 min.

[0042] III. Rapidly extrude the mixed material through a twin - screw extruder, with the extrusion temperature being 100 - 110 °C and the extruder speed being 1500 rpm.

[0043] IV. Use a cold roll and a tablet press to press and cool the extruded molten material.

[0044] V. After cooling, put the material into a grinding device to grind it into powder, thus obtaining the fire - proof insulating material.

[0045] V. Example 5 In this example, a preparation method of a fireproof and insulating material is provided, which specifically includes the following steps: I. Weigh raw materials according to the following mass fractions: Component A: Pure phenyl silicone resin SILRES® 604: 20 kg, phenolic modified epoxy resin Araldite GT 7255: 30 kg, epoxy curing agent KD405: 10 kg, isophorone diisocyanate curing agent K7150: 5 kg, acrylate leveling agent ADDITOL® P 896: 0.5 kg, PTN601: 0.2 kg, benzoin: 0.3 kg, antioxidant: 0.2 kg, flame retardant and fire-resistant functional agent DM95-G720B: 11.3 kg.

[0046] Component B: Pigment 1 kg; Filler: Glass powder: 10 kg; Mica powder: 4 kg; Aluminum phosphate: 3 kg; Wollastonite: 4.5 kg.

[0047] II. Premix the raw materials of Component A and Component B respectively, control the stirring speed during premixing at 100 - 300 rpm, and the premixing time at 2 - 10 min. Then mix Component A and Component B together, control the stirring speed during mixing at 100 rpm, and the mixing time at 5 - 10 min.

[0048] III. Rapidly extrude the mixed material through a twin-screw extruder, with the extrusion temperature at 100 - 110 °C and the extruder speed at 1500 rpm.

[0049] IV. Use a cold roll and a tablet press to press and cool the extruded molten material.

[0050] V. After cooling, put the material into a grinding equipment to grind it into powder, thus obtaining the fireproof and insulating material.

[0051] VI. Example 6 In this example, a preparation method of a fireproof and insulating material is provided, which specifically includes the following steps: I. Weigh raw materials according to the following mass fractions: Component A: Pure phenyl silicone resin SILRES® 604: 30 kg, phenolic modified epoxy resin KD211S: 20 kg, epoxy curing agent V-2051W: 7.5 kg, isophorone diisocyanate curing agent Crelan ® NW-5: 6 kg, acrylate leveling agent ADDITOL® P 896: 0.5 kg, PTN601: 0.4 kg, benzoin: 0.4 kg, antioxidant: 0.4 kg, flame retardant and fire-resistant functional agent DM95-G720B: 15 kg.

[0052] Component B: 0.8 kg of pigment; Fillers: 8 kg of glass powder; 4 kg of mica powder; 3 kg of aluminum phosphate; 4 kg of wollastonite.

[0053] II. Premix the raw materials of Component A and Component B separately, control the stirring speed during premixing at 100 - 300 rpm, and the premixing time at 2 - 10 min. Then mix Component A and Component B together, control the stirring speed during mixing at 100 rpm, and the mixing time at 5 - 10 min.

[0054] III. Rapidly extrude the mixed material through a twin - screw extruder, with the extrusion temperature at 100 - 110 °C and the extruder speed at 1500 rpm.

[0055] IV. Use a cold roll and a tablet press to press and cool the extruded molten material.

[0056] V. After cooling, put the material into a grinding equipment to grind it into powder, thus obtaining the fire - proof and insulating material.

[0057] VII. Comparative Example 1 The difference between this comparative example and Example 1 is only that the flame - retardant and fire - resistant functional agent is replaced from the DM95 - G720B raw material with commercially available magnesium hydroxide.

[0058] VIII. Comparative Example 2 The difference between this comparative example and Example 1 is only that the commercially available product of the pure phenyl silicone resin has a hydroxyl content lower than 2.5 w / w%, such as Zhejiang Hongchuang HC GT - 5, with a hydroxyl content of 2 w / w%.

[0059] IX. Comparative Example 3 The difference between this comparative example and Example 1 is only that the commercially available product of the pure phenyl silicone resin has a hydroxyl content greater than 7 w / w%, such as Changzhou Jianuo FM - CB, with a hydroxyl content of 7.5 w / w%.

[0060] Test the fire - proof and insulating materials of Examples 1 - 6 and Comparative Example 1 according to the test items, and the results are shown in Table 1.

[0061]

[0062] The flame-retardant and fire-resistant functional agent DM95-G720B used in the present invention, different from magnesium hydroxide in terms of flame-retardant and fire-resistant functions, can expand simultaneously with other fillers and remelt into a new coating film under the scenario of being burned by an open flame. The remelted and formed coating film can continue to provide insulation protection characteristics. The hydroxyl content of the silicone resin used in the present invention is 2.5 - 7 w / w%. During the curing process of the silicone resin, it can crosslink and cure with the isophorone diisocyanate curing agent, resulting in better curing degree of the coating film and better compatibility with the epoxy resin system, and the coating film has better fire-retardant and fire-resistant performance.

[0063] When the fireproof and insulating material of the present invention is used, the powder is coated on the surface of the workpiece to be protected, and the flame-retardant grade reaches UL-V0. After baking and curing, a protective coating is formed. The curing conditions are: 230 °C, 30 min; the protective coating not only has good original insulation performance, but also has good insulation effect after being burned by an open flame at 1300 °C for 30 min. Both the initial coating and the coating after being burned by an open flame can pass the insulation performance test: AC voltage 3000V, test duration 60 s, current < 1 mA. The present invention provides a fireproof and insulating material that can be spray-constructed, which can broaden the application scenarios of the product.

[0064] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements will not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A fireproof and insulating material, characterized in that, It includes raw materials with the following weight percentages: silicone resin 20 - 30%, phenol-formaldehyde modified epoxy resin 20 - 30%, epoxy curing agent 7.5 - 10%, isophorone diisocyanate curing agent 5 - 6%, leveling agent 0.5 - 1%, electrostatic charge increasing type powdering aid 0.2 - 0.5%, benzoin 0.3 - 0.5%, antioxidant 0.3 - 0.5%, flame retardant and fire-resistant functional aid 11.3 - 15%, and the balance being pigments and fillers.

2. The fireproof and insulating material according to claim 1, wherein The filler is a composition prepared from glass powder, mica powder, aluminum phosphate, and wollastonite according to the mass ratio of (8 - 10) : (4 - 5) : (2.6 - 3) : (4 - 4.5).

3. The fireproof and insulating material according to claim 1, characterized in that, The silicone resin is pure phenyl silicone resin with 100% organosilicon content and a hydroxyl content of 2.5 - 7 wt%.

4. The fireproof and insulating material according to claim 1, characterized in that, The phenol-formaldehyde modified epoxy resin has an epoxy equivalent of 750 - 900 g / eq and a viscosity of 1000 - 4000 cps / 150 °C.

5. The fireproof and insulating material according to claim 1, characterized in that, The epoxy curing agent is a resin capped with phenolic hydroxyl groups, with a hydroxyl value of 230 - 260 mgKOH / g and a softening point of 80 - 100 °C.

6. The fireproof and insulating material according to claim 1, characterized in that, The isophorone diisocyanate curing agent has an NCO value of 14 - 16 mgKOH / g and a glass transition temperature Tg of 45 - 55 °C.

7. The fireproof and insulating material according to claim 1, wherein The flame retardant and fire-resistant functional agent used is DM95-G720B sold by Amiwinas.

8. The fireproof and insulating material according to claim 1, wherein The leveling agent is an acrylate leveling agent; the electrostatic charge increasing type powdering aid is a quaternary ammonium salt type powdering aid.

9. A method for preparing a fireproof and insulating material as described in claim 1, characterized in that, It includes the following steps: S1. Premix silicone resin, phenol-formaldehyde modified epoxy resin, phenolic curing agent, isophorone diisocyanate curing agent, leveling agent, powdering aid, benzoin, antioxidant, and flame retardant and fire-resistant functional aid into component A, and premix pigments and fillers into component B; S2. After mixing component A and component B evenly, extrude at 100 - 110 °C to obtain a molten material; S3. After pressing the molten material into tablets, grind it into powder.

10. The preparation method of the fireproof and insulating material according to claim 9, characterized in that, In step S1, when premixing component A and component B, control the stirring speed at 100 - 300 rpm and the premixing time at 2 - 10 min. In step S2, when mixing component A and component B, control the stirring speed at 100 - 300 rpm and the mixing time at 2 - 10 min; the extrusion process is carried out in a twin-screw extruder, and control the speed of the twin-screw extruder at 1500 rpm.

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