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Phosphorus-containing phenolic aldehyde and preparation method thereof

A technology of phenolic and organic phosphorus, which is applied in the field of polymer compounds, can solve the problems of copper clad laminate damage, high phosphorus content, and many free phenols, and achieve good flame retardancy and heat resistance, simple preparation method, low phosphorus content, etc. high effect

Inactive Publication Date: 2010-06-02
镇江市电子化工材料工程研究中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to achieve the purpose of halogen-free flame retardant, the measures currently taken are to obtain halogen-free epoxy resin by modifying epoxy resin, and the phosphorus-containing epoxy resin can be halogen-free, but the free phenol in it is relatively Too many, the gel time is unstable, and it is easy to cause damage to materials such as copper clad laminates
In addition, the phosphorus content of phosphorus-containing epoxy resin is relatively low and cannot meet the requirements of flame retardancy, insulation, environmental protection, and mechanical properties; while the phosphorus content is high, the epoxy value is almost zero, and has no application value.

Method used

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  • Phosphorus-containing phenolic aldehyde and preparation method thereof
  • Phosphorus-containing phenolic aldehyde and preparation method thereof
  • Phosphorus-containing phenolic aldehyde and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The steps of the present embodiment are as follows: the raw material is pressed by the following weight

[0021] 9,10-dihydro-9-oxa-10phosphaphenanthrene-10 oxide 200g,

[0022] p-Hydroxybenzaldehyde 120g,

[0023] Benzenesulfonic acid 4g,

[0024] Add it into a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser, and a nitrogen inlet to stir and feed nitrogen; at the same time, the temperature is raised to 80°C, and refluxed for 8 hours to obtain a phosphorus content of 9.0% and a softening point of 100°C. Phosphorous phenolic.

[0025] The raw materials used in this example are all commercially available, and will not be repeated here.

Embodiment 2

[0027] The steps of the present embodiment are as follows: the raw material is pressed by the following weight

[0028] 2-(6H-dibenzo-5-oxa-6-phosphono-6-phenyl-1,4-hydroquinone 350g,

[0029] o-Hydroxybenzaldehyde 200g,

[0030] Benzoic acid 7g,

[0031] Add it into a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a nitrogen inlet to stir and feed nitrogen; at the same time, it is heated to 120°C and refluxed for 6 hours to obtain a phosphorus content of 9.2% and a softening point of 140°C. Phosphorous phenolic.

[0032] The raw materials used in this example are all commercially available, and will not be repeated here.

Embodiment 3

[0034] The steps of the present embodiment are as follows: the raw material is pressed by the following weight

[0035] 4-Cyclooctene containing phosphorus hydroquinone 400g,

[0036] m-Hydroxybenzaldehyde 200g,

[0037] Salicylic acid 10g,

[0038] Add it into a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a nitrogen inlet to stir and feed nitrogen; at the same time, it is heated to 150°C and refluxed for 4 hours to obtain 8.8% phosphorus content and a softening point of 150°C. Phosphorous phenolic.

[0039] The benzaldehyde and catalyzer used in the present embodiment are all available on the market, and the phosphorus-containing hydroquinone used in the present embodiment is all obtained by self-made by conventional techniques (the preparation method of epoxy resin is referring to the publication of Mechanical Industry Publishing House. Titled "Epoxy Resin Application Principles and Technologies", Section 2.4 of the second chapter, the...

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Abstract

The invention relates to a curing agent and a preparation method, in particular to a halogen-free curing agent capable of being used for curing an epoxy resin and a preparation method thereof, belonging to the technical field of the macromolecular compounds. In the invention, phosphorus element is introduced into aromatic aldehyde to form a phosphorus-containing phenolic aldehyde by modifying the curing agent and using organic phosphorus as a flame retardant, thereby the flame retardation and thermal stability of epoxy resin can be improved when in use. The invention has the advantages of simple preparation method, little pollution in the synthesis process, no poisonous gas generation in burning and no harm to human bodies. The prepared phosphorus-containing phenolic aldehyde is an environment-friendly product which has high phosphorus content, excellent flame retardation and heat-resistant property and can meet the halogen-free and lead-free requirement.

Description

technical field [0001] The invention relates to a curing agent and a preparation method thereof, in particular to a halogen-free curing agent for curing epoxy resin and a preparation method thereof, belonging to the technical field of polymer compounds. Background technique [0002] Epoxy resin composition is generally composed of epoxy resin and curing agent, and is widely used in industries such as coatings, adhesives, electronic and electrical materials, engineering plastics and composite materials. However, the obvious disadvantage of epoxy resin is that its flame retardancy is not good, and its oxygen index is only 19.8%. Halogen is usually introduced into the epoxy resin system to achieve the flame retardant effect, but when used as a flame retardant, halogen is easy to hydrolyze to produce hydrides to corrode the circuit, and produce dioxins, benzofurans and other irritants during the combustion process , Corrosive toxic gas, endangering people's health and causing e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10C08G8/20C08G59/62
Inventor 苏文国王世珍缪志杰
Owner 镇江市电子化工材料工程研究中心有限公司
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