CN112662360A

CN112662360A - Halogen-free flame-retardant polyisocyanurate foam rubber for electric appliance element packaging and preparation method thereof

Info

Publication number: CN112662360A
Application number: CN202011528112.6A
Authority: CN
Inventors: 钱建中; 钱洪祥; 冯伟; 梁舒峰; 汪乐春
Original assignee: Shanghai Huide Technology Co ltd
Current assignee: Shanghai Huide Technology Co ltd
Priority date: 2020-12-22
Filing date: 2020-12-22
Publication date: 2021-04-16
Anticipated expiration: 2040-12-22
Also published as: CN112662360B

Abstract

The invention relates to a halogen-free flame-retardant polyisocyanurate foaming adhesive for packaging electrical elements, which is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight: 30-60% of polyether polyol; 10-30% of polyester polyol; 20-40% of flame retardant; 1-3% of foam stabilizer; 1-15% of foaming agent; 1 to 2.5 percent of catalyst; 5-10% of phase-change material; the component B is polymethylene polyphenyl polyisocyanate, and the addition ratio of the component A to the component B is 100: 100-150. Its preparing process is also disclosed. The polyisocyanurate foaming adhesive disclosed by the invention is low in density, low in generated heat lower than 100 ℃, high in compressive strength, capable of achieving UL94-V0 level flame retardance and capable of being tested by alternating damp heat (12h +12h) at 25 ℃/95% -55 ℃/95% 48h, and suitable for packaging various electrical elements.

Description

Halogen-free flame-retardant polyisocyanurate foam rubber for electric appliance element packaging and preparation method thereof

Technical Field

The invention relates to the technical field of preparation of adhesive products, and particularly relates to a halogen-free flame-retardant polyisocyanurate foam adhesive for packaging electrical components and a preparation method thereof.

Background

At present, the packaging adhesives for electrical components are basically classified into epoxy, silicone and polyurethane. The basic technical requirements of the glue for electronic packaging are as follows: the adhesive force to the base material is high; the viscosity is low, and the method is suitable for encapsulation operation; the material is hydrophobic; the material has high electrical insulation; some sensors, for example, may be used in extreme air temperatures and large ambient temperature fluctuations due to complex application environments. The specific weight average of the conventional electronic pouring sealant is 1-1.1. With the rapid development of the electronic industry, electronic components are gradually developing toward miniaturization, light weight and intellectualization. The requirement for light weight packaging is also becoming more and more apparent.

Polyurethane is the most readily foamable material. The light-weight requirement of the existing electronic products can be better met. Wherein the polyisocyanurate has excellent thermal stability and flame retardancy because of no unstable hydrogen atom and high nitrogen element content in the six-membered heterocyclic ring in the structure. The specific gravity of the pouring sealant product is 0.2-0.3. The product has good sealing performance and high insulativity, has the characteristics of excellent corrosion resistance, shock resistance, damp and heat resistance, flame retardance and the like, and greatly improves the working stability and reliability of the controller.

Disclosure of Invention

The invention aims to solve the problem of changing the defects of the existing electronic packaging technology and provides polyisocyanurate foam rubber and a preparation method thereof.

By introducing trimerization reaction, halogen-free flame retardant and environment-friendly foaming agent, the environment-friendly polyisocyanurate foaming adhesive with low density, high compressive strength and low heat release is generated.

The halogen-free flame-retardant polyisocyanurate foaming adhesive for packaging the electric appliance element comprises a component A and a component B, wherein the component A comprises the following components in parts by weight:

the component B is polymethylene polyphenyl polyisocyanate, and the addition ratio of the component A to the component B is 100: 100-150.

In a preferred embodiment of the present invention, the polyether polyol is polyoxypropylene alcohol initiated with any one or more of diethylene glycol, glycerol or sucrose.

Preferably from 30% to 45% of NJ-4110A and from 0 to 15% of other polyether polyols including any one or more of NJ-305, NJ-210 or NJ-8205.

NJ-4110A is sucrose and diethylene glycol initiator, hydroxyl value is 430 +/-30 mgKOH/g, viscosity is 3400 +/-400 mPa · s; NJ-305 is a glycerol initiator, the hydroxyl value is 330 plus or minus 10mgKOH/g, and the viscosity is 300 plus or minus 70 mPa.s; NJ-210 is diethylene glycol initiator, hydroxyl value is 100 plus or minus 10mgKOH/g, viscosity is 160 plus or minus 30 mPa.s;

NJ-8205 is a sucrose and diethylene glycol initiator, with a hydroxyl value of 470 +/-30 mgKOH/g and a viscosity of 6900 +/-600 mPa.s.

In a preferred embodiment of the present invention, the polyester polyol is an aromatic polyester diol. Preferably, the aromatic polyester diol PE340 of Shanghai Huiyi science and technology Limited company has a hydroxyl value of 320 +/-10 mgKOH/g and a viscosity of 310-370 mPa.s.

In a preferred embodiment of the invention, the catalyst is any one or more of dimethylcyclohexylamine, N-dimethylbenzylamine, 1,3, 5-trihydrotriazine or a solution of potassium isooctanoate in diethylene glycol.

In a preferred embodiment of the present invention, the foam stabilizer is a silicone-based surfactant. Preferably B8450 from the German winning industry group company.

In a preferred embodiment of the invention, the blowing agent is any one or more of water, cyclopentane or isopentane.

In a preferred embodiment of the present invention, the phase change material is a non-polar wax powder with a dropping point less than 125 ℃ and a particle size less than 20 um. One or more of the Crainen Ceridust3620 and the Honeywell A-C6A are preferred.

In a preferred embodiment of the present invention, the flame retardant is any one or more of a phosphate ester additive type flame retardant, a phosphorus-containing polyol, an ammonium polyphosphate type flame retardant or an inorganic flame retardant.

Preferably any one or more of isopropylated triphenyl phosphate, resorcinol bis-diphenyl phosphate, phosphorus-containing polyols, polyphosphoric acid amines or aluminium hydroxide.

In a preferred embodiment of the present invention, the polyphenyl polymethylene isocyanate is preferably any one or more of 44V20 of bayer, germany, S5005 of hensmy chemical limited, or PM200 of cigarette taiwanese polyurethane gmbh.

A preparation method of halogen-free flame-retardant polyisocyanurate foaming adhesive for packaging electrical elements comprises the following steps:

and uniformly mixing the component A and the component B according to a proportion, putting the mixture into a high-pressure foaming machine, injecting the mixture into a mold under the conditions that the temperature of the mixture is controlled to be 3-26 ℃ and the temperature of an external mold of an electrical element is 35-40 ℃, and demolding after 10-15 minutes to obtain the halogen-free flame-retardant polyisocyanurate foaming adhesive.

In a preferred embodiment of the present invention, the overall density of the foam rubber after molding is in the range of 200-300kg/m³。

The invention has the following advantages and beneficial effects:

1. the polyurethane foaming adhesive is adopted to encapsulate the electronic material, so that the total weight is reduced. The product is lighter.

2. The invention adopts polyether polyols with high and low hydroxyl values to match, thereby reducing the heat generation of the whole reaction. And absorbs the entire heat by adding a phase change material. The whole reaction has gentle heat release, and the whole system generates heat no more than 100 ℃. The heat generation of the common foaming glue in the market exceeds 130 ℃, so that the electronic components are easily damaged, and the yield is reduced.

3. The foaming agent adopted by the invention is water and isopentane, the integral ODP and GWP values are zero, the traditional HCFC-141b foaming agent (ODP value is 0.11) is replaced, and the consumption of the ozone layer is effectively reduced

4. The flame retardant adopted by the invention is a halogen-free flame retardant, and is more environment-friendly.

Detailed Description

The technical solutions of the present invention are further described below with reference to specific examples, which are only for explaining the technical solutions of the present invention and are not used to limit the protection scope of the present invention.

Example 1

The specific components of the component A are shown in the following table 1:

TABLE 1

Name of raw materials	Number of parts
		NJ-4110A	34
NJ-210	12
		PE340	12
BDMA	1.5
		K-15	0.8
B8450	2.5
		Water (W)	0.2
Isopentane	10
		Ceridust3620	5
OP550	23

The component B is 44V20, the temperature of the mixed component A and the component B is controlled to be 23-25 ℃, the mechanical stirring speed is 4000 rpm, and the ratio of the component A to the component B is 100/130. Mixing, stirring, pouring into a mold with constant temperature of 40 deg.C, aging for 15min, and opening the mold.

And (3) standing the prepared product at normal temperature for 48 hours, and then carrying out performance test.

Example 2

The specific components of the component A are shown in the following table 2:

TABLE 2

Name of raw materials	Number of parts
		NJ-4110	40
PE340	11
		PC-41	1
K-15	1.5
		B8450	3
Water (W)	1
		A-C6A	5
AP422	20
		RDP	20

The component B is PM200, the temperature of the mixed component A and the component B is controlled to be 23-25 ℃, the mechanical stirring speed is 4000 rpm, and the ratio of the component A to the component B is 100/116.

Mixing, stirring, pouring into a mold with constant temperature of 40 deg.C, aging for 15min, and opening the mold.

Example 3

The specific components of the component A are shown in the following table 3:

TABLE 3

Name of raw materials	Number of parts
		NJ-4110A	30
PE-340	24
		K-15	1
B8450	2
		Cyclopentane	4
Isopentane	11
		A-C6A	7
Aluminum hydroxide	6
		IPPP	15

The component B is PM200, the temperature of the mixed component A and the component B is controlled to be 23-25 ℃, the mechanical stirring speed is 4000 rpm, and the ratio of the component A to the component B is 100/128.

Example 4

The specific components of the component A are shown in the following table 4:

TABLE 4

The component B is PM200, the temperature of the mixed component A and the component B is controlled to be 23-25 ℃, the mechanical stirring speed is 4000 rpm, and the ratio of the component A to the component B is 100/150.

Example 5

The specific components of the component A are shown in the following table 5:

TABLE 5

Name of raw materials	Number of parts
		NJ-4110A	47
PE340	12
		PC-41	2.5
B8450	2.5
		Water (W)	1
Cyclopentane	5
		Ceridust3620	5
IPPP	10
		OP550	15

The component B is S5005, the temperature of the mixed component A and the component B is controlled to be 23-25 ℃, the mechanical stirring speed is 4000 rpm, and the ratio of the component A to the component B is 100/100.

The results of the performance tests of the polyurethane foams prepared in examples 1-5 are shown in Table 6 below:

TABLE 6

As can be seen from tables 1-6, the polyisocyanurate foam of the invention has low density, flame retardance reaching UL94-V0 level, high compressive strength and low reaction heat generation, can pass the test of alternating damp heat (12h +12h) at 25 ℃/95% -55 ℃/95% for 48h, and is suitable for packaging various electrical elements.

Claims

1. The halogen-free flame-retardant polyisocyanurate foaming adhesive for packaging the electric appliance element is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight:

2. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the polyether polyol is polyoxypropylene alcohol using any one or more of diethylene glycol, glycerin and sucrose as an initiator.

3. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the polyester polyol is an aromatic polyester diol.

4. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the catalyst is any one or more of dimethylcyclohexylamine, N-dimethylbenzylamine, 1,3, 5-trihydrotriazine or a solution of potassium isooctanoate in diethylene glycol.

5. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the foam stabilizer is a silicone surfactant.

6. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the blowing agent is any one or more of water, cyclopentane or isopentane.

7. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the flame retardant is any one or more of phosphate additive type flame retardants, phosphorus-containing polyols, ammonium polyphosphate flame retardants or inorganic flame retardants.

8. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein the phase-change material is a low dropping point non-polar wax powder.

9. The halogen-free flame-retardant polyisocyanurate foam according to claim 1, wherein said polyphenyl polymethylene isocyanate is preferably any one or more of 44V20 from bayer, hounsfield, S5005 from hensmei chemical limited, or PM200 from nicotineak university polyurethane gmbh.

10. The method for preparing the halogen-free flame-retardant polyisocyanurate foam according to any one of claims 1 to 8, comprising the steps of:

11. The method as claimed in claim 9, wherein the molded foam has an overall density of 200-300kg/m³。