WO2019119782A1 - 用于核电或变压器无卤阻燃h级槽绝缘材料以及制备方法 - Google Patents

用于核电或变压器无卤阻燃h级槽绝缘材料以及制备方法 Download PDF

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Publication number
WO2019119782A1
WO2019119782A1 PCT/CN2018/094927 CN2018094927W WO2019119782A1 WO 2019119782 A1 WO2019119782 A1 WO 2019119782A1 CN 2018094927 W CN2018094927 W CN 2018094927W WO 2019119782 A1 WO2019119782 A1 WO 2019119782A1
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WIPO (PCT)
Prior art keywords
rubber layer
epoxy resin
flame retardant
glue
retardant
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PCT/CN2018/094927
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English (en)
French (fr)
Inventor
徐伟红
李永让
夏宇
徐芳
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苏州巨峰电气绝缘系统股份有限公司
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Publication of WO2019119782A1 publication Critical patent/WO2019119782A1/zh

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B17/00—Insulators or insulating bodies characterised by their form
    • H01B17/56—Insulating bodies
    • H01B17/60—Composite insulating bodies
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B17/00—Insulators or insulating bodies characterised by their form
    • H01B17/56—Insulating bodies
    • H01B17/66—Joining insulating bodies together, e.g. by bonding
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B19/00—Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B19/00—Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
    • H01B19/04—Treating the surfaces, e.g. applying coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/28—Coils; Windings; Conductive connections
    • H01F27/32—Insulating of coils, windings, or parts thereof
    • H01F27/324—Insulation between coil and core, between different winding sections, around the coil; Other insulation structures
    • H—ELECTRICITY
    • H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
    • H02K—DYNAMO-ELECTRIC MACHINES
    • H02K3/00—Details of windings
    • H02K3/32—Windings characterised by the shape, form or construction of the insulation
    • H02K3/34—Windings characterised by the shape, form or construction of the insulation between conductors or between conductor and core, e.g. slot insulation
    • H02K3/345—Windings characterised by the shape, form or construction of the insulation between conductors or between conductor and core, e.g. slot insulation between conductor and core, e.g. slot insulation
    • 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
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the present application belongs to the field of composite insulating materials, and particularly relates to a halogen-free flame-retardant H-stage insulating material for nuclear power or transformer, and a preparation method and application thereof.
  • the portion of the motor that forms the moving magnetic field includes the core and the coil.
  • the core has a yoke extending in a direction in which the magnetic field moves and teeth that protrude from the yoke and are arranged in the direction in which the magnetic field moves.
  • the portion between any two adjacent teeth is called a groove.
  • the coil is formed such that the wire is wound around the teeth, with the result that the coil is partially located within the slot.
  • insulating paper hereinafter referred to as slot insulating paper or groove insulating material
  • slot insulating paper or groove insulating material may be disposed along each surface of the core defining each groove.
  • NOMEX NOMEX paper
  • the purpose of the present application is to overcome the deficiencies of the prior art and provide a halogen-free flame-retardant H-stage insulating material for nuclear power or transformers with good insulation effect and environmental protection, and a preparation method and application thereof.
  • An object of the present application is to provide a halogen-free flame-retardant H-slot insulating material for nuclear power or transformer, comprising a first polyimide film layer disposed on one side of the first polyimide film layer a first mixed adhesive layer, a second mixed adhesive layer disposed on the other side of the first polyimide film layer, a first woven glass cloth disposed on the first mixed adhesive layer, and a setting a second woven glass cloth on the second mixed rubber layer, a first B-stage flame retardant rubber layer disposed on the first woven glass cloth, and disposed on the second woven glass cloth The second B-stage flame retardant layer,
  • the first B-stage flame retardant rubber layer and the second B-stage flame retardant rubber layer are formed by B-stage flame-retardant glue, and the raw materials of the B-stage flame-retardant glue respectively comprise a feed mass ratio of 10-15.
  • a halogen-free flame-retardant epoxy resin and an epoxy resin curing agent the halogen-free flame retardant epoxy resin comprising a self-flame retardant liquid epoxy resin and a self-flame retardant solid having a mass ratio of 0.5 to 2:1.
  • the liquid epoxy resin, the solid epoxy resin and the halogen-free flame retardant have a mass ratio of 0.4 to 1:0.4 to 1: 1.
  • the first B-stage flame retardant layer and the second B-stage flame retardant layer have a dry glue content of 40-60 g/m 2 , respectively .
  • the first mixed rubber layer and the second mixed rubber layer are formed by mixing glue
  • the raw materials of the mixed glue respectively include PU glue with a mass ratio of 7 to 10:1 to 1.5:1.
  • the PU glue comprises Henkel Liofol UR 2716 and Henkel curing agent UK 5500 with a mass ratio of 5-8:1, or a feed mass ratio of 6-9: 1 Bostik AP1387 and Boss Hardener Z
  • the epoxy glue comprises a modified epoxy resin and an epoxy resin curing agent with a mass ratio of 4-8:1, the modified epoxy resin It includes liquid epoxy resin and solid epoxy resin with a feed mass ratio of 0.5 to 2:1.
  • the liquid epoxy resin and the solid epoxy resin have a mass ratio of 0.8 to 1.2:1.
  • the first mixed rubber layer and the second mixed rubber layer have a dry glue content of 10-20 g/m 2 , respectively .
  • the halogen-free flame-retardant H-slot insulating material further comprises a third mixed adhesive layer disposed between the first woven glass cloth and the first B-stage flame retardant rubber layer, and is disposed at a second polyimide film layer between the third mixed rubber layer and the first B-stage flame retardant layer, the second polyimide film layer and the first a fourth mixed rubber layer between the B-stage flame retardant rubber layers, and a third woven glass cloth disposed between the fourth mixed rubber layer and the first B-stage flame retardant rubber layer.
  • the third mixed rubber layer and the fourth mixed rubber layer are formed by mixing glue
  • the raw materials of the mixed glue respectively include PU with a mass ratio of 7 to 10:1 to 1.5:1.
  • Glue, epoxy glue and halogen-free flame retardant the PU glue comprises Henkel Liofol UR 2716 and Henkel curing agent UK 5500 with a mass ratio of 5-8:1, or a feed mass ratio of 6-9 : 1 Bostik AP1387 and Boss Hardener Z;
  • the epoxy adhesive comprises a modified epoxy resin and an epoxy resin curing agent having a mass ratio of 4 to 8:1, the modified epoxy
  • the resin includes a liquid epoxy resin and a solid epoxy resin having a feed mass ratio of 0.5 to 2:1.
  • the liquid epoxy resin and the solid epoxy resin have a mass ratio of 0.8 to 1.2:1.
  • the third mixed rubber layer and the fourth mixed rubber layer have a dry glue content of 10-20 g/m 2 , respectively .
  • Another object of the present application is to provide a method for preparing a halogen-free flame retardant H-stage insulating material for nuclear power or transformer, comprising the following steps:
  • Step (1) mixing the double-sided glue of the first polyimide film, and then removing the solvent at 70-100 ° C, a vehicle speed of 10 ⁇ 3 m / min, and a tension of 60 - 80 N.
  • Step (2) compounding a woven glass cloth on the first mixed rubber layer and the second mixed rubber layer to form the first woven glass cloth and the second woven glass cloth, and then winding, winding
  • the material is cured at 120 ⁇ 5 ° C for 20 to 30 hours;
  • Step (3) the B-stage flame-retardant glue on the surface of the first woven glass cloth and the second woven glass cloth, and then drying in an oven to an epoxy resin to reach a B-stage, forming The first B-stage flame retardant rubber layer and the second B-stage flame retardant rubber layer, wherein the temperature of the front end of the oven is controlled to be 80-100 ° C, and the temperature of the middle and rear sections is 130-150 °C.
  • a third object of the present application is to provide a method for preparing a halogen-free flame retardant H-stage insulating material for nuclear power or transformer, comprising the following steps:
  • Step (1) mixing the double-sided glue of the first polyimide film, and then removing the solvent at 70-100 ° C, a vehicle speed of 10 ⁇ 3 m / min, and a tension of 60 - 80 N.
  • Step (2) compounding a woven glass cloth on the first mixed rubber layer and the second mixed rubber layer to form the first woven glass cloth and the second woven glass cloth, and then winding, winding
  • the material is cured at 120 ⁇ 5 ° C for 20 to 30 hours;
  • Step (3) mixing the glue on one side of the second polyimide film, and then removing the solvent at 70 to 100 ° C, a vehicle speed of 10 ⁇ 3 m / min, and a tension of 60 to 80 N to obtain the first Four mixed rubber layers;
  • Step (4) compounding a woven glass cloth on the fourth mixed rubber layer to form a third woven glass cloth
  • Step (5) mixing glue on the other side of the second polyimide film, and then removing the solvent at 70 to 100 ° C to form a third mixed rubber layer at a speed of 15 ⁇ 3 m / min, tension Coordinating the third mixed rubber layer with the first woven glass cloth at 70-90N;
  • Step (6) the B-stage flame-retardant glue on the surface of the third woven glass cloth and the second woven glass cloth, and then drying in an oven to the epoxy resin to reach the B-stage, forming The first B-stage flame retardant rubber layer and the second B-stage flame retardant rubber layer, wherein the temperature of the front end of the oven is controlled to be 80-100 ° C, and the temperature of the middle and rear sections is 130-150 °C.
  • a fourth object of the present application is to provide an application of the halogen-free flame-retardant H-stage insulating material in a power generating rotor tank for nuclear power or transformers.
  • the epoxy resin curing agent is a mixture of one or more selected from the group consisting of aromatic diamine curing agents, and the liquid epoxy resin is E44-6101, the solid ring.
  • the oxygen resin is E12-604, and the halogen-free flame retardant is one or a mixture of dimethyl methyl phosphate, low poly ammonium polyphosphate and triphenyl phosphate.
  • the aromatic diamine curing agent includes diaminodiphenyl sulfone (DDS), diaminodiphenylmethane (DDM), m-phenylenediamine (MPDA), 4,4' diaminodiphenyl ether ( DDE) and p-xylyleneamine (DMB) and the like.
  • DDS diaminodiphenyl sulfone
  • DDM diaminodiphenylmethane
  • MPDA m-phenylenediamine
  • DDE 4,4' diaminodiphenyl ether
  • DMB p-xylyleneamine
  • the self-flame retardant liquid epoxy resin and the self-flame-retardant solid epoxy resin may also be a conventional flame retardant epoxy resin containing P, N, such as olfactory epoxy.
  • the mixed glue is prepared by adding the liquid epoxy resin and the solid epoxy resin to a solvent, stirring for 30 ⁇ 5 minutes, and then adding the epoxy resin to cure. Stirring for 10 ⁇ 5 minutes, adding the halogen-free flame retardant, stirring for 10 ⁇ 5 minutes, adding a component of the PU glue, stirring for 20 ⁇ 5 minutes, adding the PU glue. The other ingredient was stirred for 10 ⁇ 5 minutes, and then the viscosity of the mixed glue of 20 to 30 ° C 4 # cup was adjusted to 15-16 seconds with a solvent.
  • the group distribution ratio of the mixed glue can improve the tensile strength and insulation properties of the product.
  • the B-stage flame-retardant glue is prepared by adding the liquid epoxy resin and the solid epoxy resin to a solvent, stirring for 30 ⁇ 5 minutes, and then adding the ring.
  • Oxygen resin curing agent stirring for 10 ⁇ 5 minutes, then adding the halogen-free flame retardant, stirring for 10 ⁇ 5 minutes;
  • the solvent is ethyl acetate, methyl ethyl ketone or acetone.
  • the thickness of the insulating material of the present application can be freely combined and matched according to the use requirements.
  • the application adopts the B-stage flame-retardant glue and the mixed glue, and through the multi-layer composite of the polyimide film and the woven glass cloth, the insulating material is not easy to absorb moisture, the insulation effect is good, and the temperature resistance level can reach the H level.
  • the preparation methods of the examples 1 to 4 are as follows.
  • the mixing ratio of the mixed glue is shown in Table 1.
  • the proportion of the B-stage flame-retardant glue is shown in Table 2.
  • the properties of the product are shown in Table 3.
  • Step (1) preparing mixed glue: adding liquid epoxy resin E44-6101 and solid epoxy resin E12-604 to acetone, stirring for 30 ⁇ 5 minutes, then adding epoxy resin curing agent, stirring for 10 ⁇ 5 minutes, Add a halogen-free flame retardant, stir for 10 ⁇ 5 minutes, add a component of PU glue (UR 2716 or AP1387), stir for 20 ⁇ 5 minutes, add another component in PU glue (UK 5500 or Hardener Z ), stir for 10 ⁇ 5 minutes, then adjust the viscosity of the 25 ° C 4 # cup of the mixed glue to 15-16 seconds with acetone.
  • PU glue UR 2716 or AP1387
  • Step (2) preparing B-stage flame retardant glue: adding liquid epoxy resin E44-6101 and solid epoxy resin E12-604 to acetone, stirring for 30 ⁇ 5 minutes, then adding epoxy resin curing agent, stirring 10 ⁇ After 5 minutes, add a halogen-free flame retardant and stir for 10 ⁇ 5 minutes.
  • Step (3) mixing the double-sided glue on the polyimide film, and then removing the solvent at 80 ° C, a vehicle speed of 10 ⁇ 3 m / min, and a tension of 70 N to obtain a first mixed rubber layer and a second mixed rubber Floor;
  • Step (4) compounding the woven glass cloth on the first mixed rubber layer and the second mixed rubber layer to form the first woven glass cloth and the second woven glass cloth, and then winding, and the coil is cured at 120 ⁇ 5° C. 24 hour;
  • Step (5) B-stage flame-retardant glue on the surface of the first woven glass cloth and the second woven glass cloth, and then dried in an oven to the epoxy resin to reach the B-stage to form the first B-stage flame retardant rubber layer and The second B-stage flame retardant layer, wherein the temperature of the front end of the control oven is 90 ° C, and the temperature of the middle section and the back section is 140 ° C.
  • the mixing ratio of the mixed glue is shown in Table 1.
  • the proportion of the B-stage flame retardant glue is shown in Table 2.
  • the performance of the product is shown in Table 3.
  • the formulation of the mixed glue and the preparation of the B-stage flame retardant glue were the same as in Example 1.
  • Step (1) mixing the double-sided glue of the polyimide film, and then removing the solvent at 80 ° C, a vehicle speed of 10 ⁇ 3 m / min, and a tension of 70 N to obtain a first mixed rubber layer and a second mixed rubber Floor;
  • Step (2) compounding the woven glass cloth on the first mixed rubber layer and the second mixed rubber layer to form the first woven glass cloth and the second woven glass cloth, and then winding, and the coil is cured at 120 ⁇ 5° C. 24 hour;
  • Step (3) mixing the glue on one side of the second polyimide film, and then removing the solvent at 80 ° C, a vehicle speed of 10 ⁇ 3 m / min, and a tension of 70 N to obtain a fourth mixed rubber layer;
  • Step (4) compounding a woven glass cloth on the fourth mixed rubber layer to form a third woven glass cloth
  • Step (5) mixing glue on the other side of the second polyimide film, and then removing the solvent at 80 ° C to form a third mixed rubber layer, which will be at a speed of 15 ⁇ 3 m / min and a tension of 80 N
  • the three mixed rubber layers are composited with the first woven glass cloth;
  • Step (6) B-stage flame retardant glue on the surface of the third woven glass cloth and the second woven glass cloth, and then dried in an oven to the epoxy resin to reach the B step, forming the first B-stage flame retardant rubber layer and The second B-stage flame retardant layer, wherein the temperature of the front end of the control oven is 90 ° C, and the temperature of the middle section and the back section is 140 ° C.
  • the preparation method was the same as that of Example 1, except that the B-stage flame-retardant glue used the mixed glue of Example 1, that is, the rubber layers in Comparative Example 3 were all formed by the mixed glue.
  • Product performance is shown in Table 3.
  • the preparation method is the same as that of the first embodiment, except that the mixed glue is formed by using the B-stage flame-retardant glue of the first embodiment, that is, the rubber layer uniform B-stage flame-retardant glue in the comparative example 4.
  • Product performance is shown in Table 3.
  • Curing conditions are recommended: 130 ° C for 5 hours; or 140 ° C for 4 hours; or 150 ° C for 3 hours.
  • the nominal thickness, the tensile strength is not bent, the breakdown voltage is not bent, the temperature index TI, the flame retardant grade, the amount of glue absorption test method refers to GBT5591.2-2002 soft composite material for electrical insulation Part 2: experiment method.
  • the test method for moisture absorption rate refers to GBT1034-2008.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Insulating Bodies (AREA)
  • Laminated Bodies (AREA)
  • Insulation, Fastening Of Motor, Generator Windings (AREA)

Abstract

本申请涉及一种用于核电或变压器无卤阻燃H级槽绝缘材料，包括第一聚酰亚胺薄膜层、第一混合胶层、第二混合胶层、第一编织玻璃布、第二编织玻璃布、第一B阶阻燃胶层、第二B阶阻燃胶层，第一B阶阻燃胶层和第二B阶阻燃胶层由B阶阻燃胶水形成，B阶阻燃胶水的原料分别包括投料质量比为10～15:1的无卤阻燃环氧树脂和环氧树脂固化剂，无卤阻燃环氧树脂包括投料质量比为0.5～2:1的自阻燃液体环氧树脂和自阻燃固体环氧树脂，或者包括投料质量比为0.4～2:0.4～2:1的液体环氧树脂、固体环氧树脂和无卤阻燃剂。本申请的绝缘材料不容易吸潮、绝缘效果好，耐温等级能够达到H级。

Description

用于核电或变压器无卤阻燃H级槽绝缘材料以及制备方法 技术领域
本申请属于复合绝缘材料领域，具体涉及一种用于核电或变压器无卤阻燃H级槽绝缘材料以及制备方法和应用。
背景技术
电动机形成移动磁场的部分包括铁心和线圈。铁心具有沿磁场移动的方向延伸的磁轭和从磁轭突出并且沿磁场移动方向排列的齿。任何相邻的两个齿之间的部分称为槽。线圈形成为使得导线卷绕在齿周围，结果线圈部分地位于槽内。为了确保电动机的铁心和线圈之间的电绝缘，可沿铁心的限定各槽的各表面配置绝缘纸(在下文中称作槽绝缘纸或者槽绝缘材料)。
现有核电或变压器用发电机转子槽内绝缘件，由于结构等原因，诺梅克斯(NOMEX纸)外置，容易吸潮，边口容易向内变形，不能很好起到绝缘保护作用。
申请内容
本申请目的是为了克服现有技术的不足而提供一种绝缘效果好且绿色环保的用于核电或变压器无卤阻燃H级槽绝缘材料以及制备方法和应用。
为达到上述目的，本申请采用的技术方案是：
本申请的一个目的是提供一种用于核电或变压器无卤阻燃H级槽绝缘材料，包括第一聚酰亚胺薄膜层、设置在所述的第一聚酰亚胺薄膜层的一面上的第一混合胶层、设置在所述的第一聚酰亚胺薄膜层的另一面上的第二混合胶层、设置在所述的第一混合胶层上的第一编织玻璃布、设置在所述的第二混合胶层上的第二编织玻璃布、设置在所述的第一编织玻璃布上的第一B阶阻燃胶层、设置在所述的第二编织玻璃布上的第二B阶阻燃胶层，
所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层由B阶阻燃胶水形成，所述的B阶阻燃胶水的原料分别包括投料质量比为10～15:1的无卤阻燃环氧树脂和环氧树脂固化剂，所述的无卤阻燃环氧树脂包括投料质量比为0.5～2:1的自阻燃液体环氧树脂和自阻燃固体环氧树脂，或者包括投料质量比为0.4～2:0.4～2:1的液体环氧树脂、固体环氧树脂和无卤阻燃剂。
优选地，所述的B阶阻燃胶水中，所述的液体环氧树脂、所述的固体环氧树脂和所述的无卤阻燃剂的投料质量比为0.4～1:0.4～1:1。
优选地，所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层的干胶含量分别为40～60g/m 2。
优选地，所述的第一混合胶层和所述的第二混合胶层由混合胶水形成，所述的混合胶水的原料分别包括投料质量比为7～10:1～1.5:1的PU胶、环氧胶和无卤阻燃剂，所述的PU胶包括投料质量比为5～8:1的汉高Liofol UR 2716和汉高固化剂UK 5500，或者包括投料质量比为6～9:1的波士胶AP1387和波士胶Hardener Z；所述的环氧胶包括投料质量比为4～8:1的改性环氧树脂和环氧树脂固化剂，所述的改性环氧树脂包括投料质量比为0.5～2:1的液体环氧树脂和固体环氧树脂。
进一步优选地，所述的混合胶水中，所述的液体环氧树脂和所述的固体环氧树脂的投料质量比为0.8～1.2:1。
优选地，所述的第一混合胶层和所述的第二混合胶层的干胶含量分别为10～20g/m 2。
优选地，所述的无卤阻燃H级槽绝缘材料还包括设置在所述的第一编织玻璃布和所述的第一B阶阻燃胶层之间的第三混合胶层、设置在所述的第三混合胶层和所述的第一B阶阻燃胶层之间的第二聚酰亚胺薄膜层、设置在所述的第二聚酰亚胺薄膜层和所述的第一B阶阻燃胶层之间的第四混合胶层、设置在所述的第四混合胶层和所述的第一B阶阻燃胶层之间的第三编织玻璃布。
进一步优选地，所述的第三混合胶层和所述的第四混合胶层由混合胶水形成，所述的混合胶水的原料分别包括投料质量比为7～10:1～1.5:1的PU胶、环氧胶和无卤阻燃剂，所述的PU胶包括投料质量比为5～8:1的汉高Liofol UR 2716和汉高固化剂UK 5500，或者包括投料质量比为6～9:1的波士胶AP1387和波士胶Hardener Z；所述的环氧胶包括投料质量比为4～8:1的改性环氧树脂和环氧树脂固化剂，所述的改性环氧树脂包括投料质量比为0.5～2:1的液体环氧树脂和固体环氧树脂。
更为优选地，所述的混合胶水中，所述的液体环氧树脂和所述的固体环氧树脂的投料质量比为0.8～1.2:1。
进一步优选地，所述的第三混合胶层和所述的第四混合胶层的干胶含量分别为10～20g/m 2。
本申请的另一个目的是提供一种所述的用于核电或变压器无卤阻燃H级槽绝缘材料的制备方法，包括如下步骤：
步骤(1)、将所述的第一聚酰亚胺薄膜的双面上混合胶水，然后在70～100℃、车速为10±3米/分钟、张力为60～80N下除溶剂，得到所述的第一混合胶层和所述的第二混合胶层；
步骤(2)、在所述的第一混合胶层和所述的第二混合胶层上复合编织玻璃布，形成所述的第一编织玻璃布和第二编织玻璃布，然后收卷，卷材在120±5℃下固化20～30小时；
步骤(3)、在所述的第一编织玻璃布和所述的第二编织玻璃布的表面上所述的B阶阻燃 胶水，然后在烘箱中烘干至环氧树脂达到B阶，形成所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层，其中，控制所述的烘箱前端的温度为80-100℃、中段和后段的温度为130～150℃。
本申请的第三个目的是提供一种所述的用于核电或变压器无卤阻燃H级槽绝缘材料的制备方法，包括如下步骤：
步骤(1)、将所述的第一聚酰亚胺薄膜的双面上混合胶水，然后在70～100℃、车速为10±3米/分钟、张力为60～80N下除溶剂，得到所述的第一混合胶层和所述的第二混合胶层；
步骤(2)、在所述的第一混合胶层和所述的第二混合胶层上复合编织玻璃布，形成所述的第一编织玻璃布和第二编织玻璃布，然后收卷，卷材在120±5℃下固化20～30小时；
步骤(3)、将所述的第二聚酰亚胺薄膜的单面上混合胶水，然后在70～100℃、车速为10±3米/分钟、张力为60～80N下除溶剂，得到第四混合胶层；
步骤(4)、在所述的第四混合胶层上复合编织玻璃布，形成第三编织玻璃布；
步骤(5)、在所述的第二聚酰亚胺薄膜的另一面上混合胶水，然后在70～100℃除溶剂，形成第三混合胶层，在车速为15±3米/分钟、张力为70～90N下将所述的第三混合胶层与所述的第一编织玻璃布复合；
步骤(6)、在所述的第三编织玻璃布和所述的第二编织玻璃布的表面上所述的B阶阻燃胶水，然后在烘箱中烘干至环氧树脂达到B阶，形成所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层，其中，控制所述的烘箱前端的温度为80-100℃、中段和后段的温度为130～150℃。
本申请的第四个目的是提供一种所述的无卤阻燃H级槽绝缘材料在核电或变压器用发电转子槽中的应用。
本申请中，所述的环氧树脂固化剂为选自芳香族二胺类固化剂中的一种或多种组成的混合物，所述的液体环氧树脂为E44-6101，所述的固体环氧树脂为E12-604，所述的无卤阻燃剂为甲基磷酸二甲酯、低聚聚磷酸铵和磷酸三苯酯中的一种或混合物。
进一步优选地，芳香族二胺类固化剂包括二胺基二苯砜(DDS)、二胺基二苯甲烷(DDM)、间苯二胺(MPDA)、4,4’二氨基二苯醚(DDE)和对二甲苯胺(DMB)等。
优选地，自阻燃液体环氧树脂和自阻燃固体环氧树脂也可以采用现有含P，N的阻燃环氧树脂，如嗅环氧等。
本申请中，所述的混合胶水的制备方法为：将所述的液体环氧树脂和所述的固体环氧树脂加入到溶剂中，搅拌30±5分钟，然后加入所述的环氧树脂固化剂，搅拌10±5分钟，再加入所述的无卤阻燃剂，搅拌10±5分钟，加入所述的PU胶中的一种成分，搅拌20±5分 钟，加入所述的PU胶中的另一种成分，搅拌10±5分钟，然后用溶剂将混合胶水的20～30℃4#杯粘度调整到15-16秒。
本申请中，混合胶水的组分配比能够提高产品的拉伸强度和绝缘性能。
本申请中，所述的B阶阻燃胶水的制备方法为：将所述的液体环氧树脂和所述的固体环氧树脂加入到溶剂中，搅拌30±5分钟，然后加入所述的环氧树脂固化剂，搅拌10±5分钟，再加入所述的无卤阻燃剂，搅拌10±5分钟；
其中，所述的溶剂为醋酸乙酯、甲乙酮或丙酮。
本申请的绝缘材料的厚度可根据使用要求进行自由组合搭配。
由于上述技术方案运用，本申请与现有技术相比具有下列优点：
本申请通过采用B阶阻燃胶水和混合胶水，并通过聚酰亚胺薄膜和编织玻璃布的多层复合，使得绝缘材料不容易吸潮、绝缘效果好，耐温等级能够达到H级。
具体实施方式
下面将结合实施例对本申请进行进一步说明。
实施例1至4各实施例的制备方法如下，混合胶水的配比见表1，B阶阻燃胶水的配比见表2，产品的性能见表3。
制备方法：
步骤(1)、配制混合胶水：将液体环氧树脂E44-6101和固体环氧树脂E12-604加入到丙酮中，搅拌30±5分钟，然后加入环氧树脂固化剂，搅拌10±5分钟，再加入无卤阻燃剂，搅拌10±5分钟，加入PU胶中的一种成分(UR 2716或AP1387)，搅拌20±5分钟，加入PU胶中的另一种成分(UK 5500或Hardener Z)，搅拌10±5分钟，然后用丙酮将混合胶水的25℃4#杯粘度调整到15-16秒。
步骤(2)、配制B阶阻燃胶水：将液体环氧树脂E44-6101和固体环氧树脂E12-604加入到丙酮中，搅拌30±5分钟，然后加入环氧树脂固化剂，搅拌10±5分钟，再加入无卤阻燃剂，搅拌10±5分钟。
步骤(3)、将聚酰亚胺薄膜的双面上混合胶水，然后在80℃、车速为10±3米/分钟、张力为70N下除溶剂，得到第一混合胶层和第二混合胶层；
步骤(4)、在第一混合胶层和第二混合胶层上复合编织玻璃布，形成第一编织玻璃布和第二编织玻璃布，然后收卷，卷材在120±5℃下固化24小时；
步骤(5)、在第一编织玻璃布和第二编织玻璃布的表面上B阶阻燃胶水，然后在烘箱中烘干至环氧树脂达到B阶，形成第一B阶阻燃胶层和第二B阶阻燃胶层，其中，控制烘箱 前端的温度为90℃、中段和后段的温度为140℃。
实施例5
混合胶水的配比见表1，B阶阻燃胶水的配比见表2，产品的性能见表3。混合胶水的配制和B阶阻燃胶水的配制同实施例1。
制备方法：
步骤(1)、将聚酰亚胺薄膜的双面上混合胶水，然后在80℃、车速为10±3米/分钟、张力为70N下除溶剂，得到第一混合胶层和第二混合胶层；
步骤(2)、在第一混合胶层和第二混合胶层上复合编织玻璃布，形成第一编织玻璃布和第二编织玻璃布，然后收卷，卷材在120±5℃下固化24小时；
步骤(3)、将第二聚酰亚胺薄膜的单面上混合胶水，然后在80℃、车速为10±3米/分钟、张力为70N下除溶剂，得到第四混合胶层；
步骤(4)、在第四混合胶层上复合编织玻璃布，形成第三编织玻璃布；
步骤(5)、在第二聚酰亚胺薄膜的另一面上混合胶水，然后在80℃除溶剂，形成第三混合胶层，在车速为15±3米/分钟、张力为80N下将第三混合胶层与第一编织玻璃布复合；
步骤(6)、在第三编织玻璃布和第二编织玻璃布的表面上B阶阻燃胶水，然后在烘箱中烘干至环氧树脂达到B阶，形成第一B阶阻燃胶层和第二B阶阻燃胶层，其中，控制烘箱前端的温度为90℃、中段和后段的温度为140℃。
表1
Figure PCTCN2018094927-appb-000001
Figure PCTCN2018094927-appb-000002
表2
Figure PCTCN2018094927-appb-000003
对比例1
基本上与实施例1相同，不同之处在于：采用诺梅克斯纸代替编织玻璃布。
对比例2
制备方法与实施例1相同，不同之处在于，B阶阻燃胶水采用实施例1的混合胶水，即对比例3中的胶层均由混合胶水形成。产品的性能见表3
对比例3
制备方法与实施例1相同，不同之处在于，混合胶水采用实施例1的B阶阻燃胶水，即对比例4中的胶层均匀B阶阻燃胶水形成。产品的性能见表3
表3
Figure PCTCN2018094927-appb-000004
Figure PCTCN2018094927-appb-000005
推荐固化条件：130℃ 5小时；或140℃ 4小时；或150℃ 3小时。
其中，标称厚度、拉伸强度不弯折、击穿电压不弯折、温度指数TI、阻燃等级、吸胶量的测试方法参照GBT5591.2-2002电气绝缘用柔软复合材料第2部分：试验方法。
吸湿率的测试方法参照GBT1034-2008。
上述实施例只为说明本申请的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本申请的内容并据以实施，并不能以此限制本申请的保护范围，凡根据本申请精神实质所作的等效变化或修饰，都应涵盖在本申请的保护范围之内。

Claims (10)

  1. 一种用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：包括第一聚酰亚胺薄膜层、设置在所述的第一聚酰亚胺薄膜层的一面上的第一混合胶层、设置在所述的第一聚酰亚胺薄膜层的另一面上的第二混合胶层、设置在所述的第一混合胶层上的第一编织玻璃布、设置在所述的第二混合胶层上的第二编织玻璃布、设置在所述的第一编织玻璃布上的第一B阶阻燃胶层、设置在所述的第二编织玻璃布上的第二B阶阻燃胶层，
    所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层由B阶阻燃胶水形成，所述的B阶阻燃胶水的原料分别包括投料质量比为10～15:1的无卤阻燃环氧树脂和环氧树脂固化剂，所述的无卤阻燃环氧树脂包括投料质量比为0.5～2:1的自阻燃液体环氧树脂和自阻燃固体环氧树脂，或者包括投料质量比为0.4～2:0.4～2:1的液体环氧树脂、固体环氧树脂和无卤阻燃剂。
  2. 根据权利要求1所述的用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层的干胶含量分别为40～60g/m 2。
  3. 根据权利要求1所述的用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：所述的第一混合胶层和所述的第二混合胶层由混合胶水形成，所述的混合胶水的原料分别包括投料质量比为7～10:1～1.5:1的PU胶、环氧胶和无卤阻燃剂，所述的PU胶包括投料质量比为5～8:1的汉高Liofol UR 2716和汉高固化剂UK 5500，或者包括投料质量比为6～9:1的波士胶AP1387和波士胶Hardener Z；所述的环氧胶包括投料质量比为4～8:1的改性环氧树脂和环氧树脂固化剂，所述的改性环氧树脂包括投料质量比为0.5～2:1的液体环氧树脂和固体环氧树脂。
  4. 根据权利要求1或3所述的用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：所述的第一混合胶层和所述的第二混合胶层的干胶含量分别为10～20g/m 2。
  5. 根据权利要求1至3中任一项所述的用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：所述的无卤阻燃H级槽绝缘材料还包括设置在所述的第一编织玻璃布和所述的第一B阶阻燃胶层之间的第三混合胶层、设置在所述的第三混合胶层和所述的第一B阶阻燃胶层之间的第二聚酰亚胺薄膜层、设置在所述的第二聚酰亚胺薄膜层和所述的第一B阶阻燃胶层之间的第四混合胶层、设置在所述的第四混合胶层和所述的第一B阶阻燃胶层之间的第三编织玻璃布。
  6. 根据权利要求5所述的用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：所述的第三混合胶层和所述的第四混合胶层由混合胶水形成，所述的混合胶水的原料分别包括投料质量比为7～10:1～1.5:1的PU胶、环氧胶和无卤阻燃剂，所述的PU胶包括投料质量比为5～8:1的汉高Liofol UR 2716和汉高固化剂UK 5500，或者包括投料质量比 为6～9:1的波士胶AP1387和波士胶Hardener Z；所述的环氧胶包括投料质量比为4～8:1的改性环氧树脂和环氧树脂固化剂，所述的改性环氧树脂包括投料质量比为0.5～2:1的液体环氧树脂和固体环氧树脂。
  7. 根据权利要求6所述的用于核电或变压器无卤阻燃H级槽绝缘材料，其特征在于：所述的第三混合胶层和所述的第四混合胶层的干胶含量分别为10～20g/m 2。
  8. 一种如权利要求1至4中任一项所述的用于核电或变压器无卤阻燃H级槽绝缘材料的制备方法，其特征在于：包括如下步骤：
    步骤(1)、将所述的第一聚酰亚胺薄膜的双面上混合胶水，然后在70～100℃、车速为10±3米/分钟、张力为60～80N下除溶剂，得到所述的第一混合胶层和所述的第二混合胶层；
    步骤(2)、在所述的第一混合胶层和所述的第二混合胶层上复合编织玻璃布，形成所述的第一编织玻璃布和第二编织玻璃布，然后收卷，卷材在120±5℃下固化20～30小时；
    步骤(3)、在所述的第一编织玻璃布和所述的第二编织玻璃布的表面上所述的B阶阻燃胶水，然后在烘箱中烘干至环氧树脂达到B阶，形成所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层，其中，控制所述的烘箱前端的温度为80-100℃、中段和后段的温度为130～150℃。
  9. 一种如权利要求5至7中任一项所述的用于核电或变压器无卤阻燃H级槽绝缘材料的制备方法，其特征在于：包括如下步骤：
    步骤(1)、将所述的第一聚酰亚胺薄膜的双面上混合胶水，然后在70～100℃、车速为10±3米/分钟、张力为60～80N下除溶剂，得到所述的第一混合胶层和所述的第二混合胶层；
    步骤(2)、在所述的第一混合胶层和所述的第二混合胶层上复合编织玻璃布，形成所述的第一编织玻璃布和第二编织玻璃布，然后收卷，卷材在120±5℃下固化20～30小时；
    步骤(3)、将所述的第二聚酰亚胺薄膜的单面上混合胶水，然后在70～100℃、车速为10±3米/分钟、张力为60～80N下除溶剂，得到第四混合胶层；
    步骤(4)、在所述的第四混合胶层上复合编织玻璃布，形成第三编织玻璃布；
    步骤(5)、在所述的第二聚酰亚胺薄膜的另一面上混合胶水，然后在70～100℃除溶剂，形成第三混合胶层，在车速为15±3米/分钟、张力为70～90N下将所述的第三混合胶层与所述的第一编织玻璃布复合；
    步骤(6)、在所述的第三编织玻璃布和所述的第二编织玻璃布的表面上所述的B阶阻燃胶水，然后在烘箱中烘干至环氧树脂达到B阶，形成所述的第一B阶阻燃胶层和所述的第二B阶阻燃胶层，其中，控制所述的烘箱前端的温度为80-100℃、中段和后段的温度为130～150℃。
  10. 一种如权利要求1至7中任一项所述的无卤阻燃H级槽绝缘材料在核电或变压器用发电转子槽中的应用。
PCT/CN2018/094927 2017-12-22 2018-07-07 用于核电或变压器无卤阻燃h级槽绝缘材料以及制备方法 WO2019119782A1 (zh)

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