Linetype bisphenol F phenolic resin and preparation method thereof

A phenolic resin and novolac bisphenol technology, applied to the field of in-line bisphenol F phenolic resin and its preparation, can solve the problems such as the influence of the internal quality of printed circuit boards, the reduction of impact resistance, and the influence of the appearance quality of printed circuit boards.

Inactive Publication Date: 2008-01-02
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But they all have disadvantages: (1) Novolak phenolic resin mainly shows that the existence of free phenol in the resin will cause the product itself to have a darker color, and the color of the cured product will often be further deepened under the heating process conditions during processing. problem, which directly affects the appearance quality of printed circuit boards
At the same time, what is more serious is that free phenol also leads to the decline of the overall performance of the cured product, which has a greater impact on the internal quality of the printed circuit board; (2) bisphenol A is used to replace monofunctional phenol in the synthesis of novolac bisphenol A phenolic resin, There is no problem of free phenol, the synthetic resin is light in color and stable, and the obtained resin product can overcome the deficiency of the novolak phenolic resin as the curing agent for epoxy copper-clad printed circuit laminates, but the novolac bisphenol A phenolic resin It can be seen from the structure that the isopropyl structure in the bisphenol A molecule restricts the rotation of the chain, thus making the molecular chain more rigid, which will lead to a decrease in the impact resistance of the system

Method used

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  • Linetype bisphenol F phenolic resin and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: Add 188g of raw material phenol, 138.4g of phosphoric acid with a mass fraction of 85%, and 50g of water into a 1000ml three-neck flask equipped with a thermometer, a stirrer, and a constant pressure dropping funnel according to the proportioning ratio. Start the agitator to mix evenly, then raise the temperature to 35°C±2°C, add 32.4g of formaldehyde with a mass fraction of 37% dropwise at a constant speed within 6 hours, add 80g of methyl isobutyl ketone to extract bisphenol F, phenol and acid A mixture of water, separate the mixture containing phosphoric acid and water in the lower layer for recycling, wash the product with distilled water until the pH is 7, vacuum dehydrate and solvent at 100 ° C ~ 140 ° C, -0.06 MPa ~ -0.09 MPa, and The excess phenol was recovered to obtain bisphenol F as a white solid.

[0029] Step 2: In 70.4g of bisphenol F, add 20g of formaldehyde with a mass fraction of 37%, 0.8g of oxalic acid, 1g of hydrochloric acid and 100g of wate...

Embodiment 2

[0041] Add 188g of raw material phenol, 115.3g of phosphoric acid with a mass fraction of 85%, and 27.0g of water into a 1000ml three-necked flask equipped with a thermometer, a stirrer, and a constant pressure dropping funnel, start the stirrer to mix evenly, and then raise the temperature to To 50°C±2°C, add 54.1g of formaldehyde with a mass fraction of 37% dropwise within 4 hours at a constant speed, add 100g of methyl isobutyl ketone to extract bisphenol F, and separate the mixture of phosphoric acid and water in the lower layer for recycling. Wash the product with distilled water until the pH is 7, carry out vacuum dehydration and solvent at 100~140°C, -0.06MPa~-0.09MPa, and recover excess phenol to obtain white solid bisphenol F.

[0042] Step 2: Add 39.3g of formaldehyde with a mass fraction of 37%, 1.5g of oxalic acid, 0.5g of hydrochloric acid and 130g of water to 113.9g of bisphenol F and heat it up to 80°C±2°C for 3 hours to stop the reaction. Suck out the acid solu...

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Abstract

The invention relates to a method for preparing a linear bisphenol F formaldehyde-phenol resin, which is characterized by the following: synthesizing the bisphenol F firstly; synthesizing bisphenol F formaldehyde-phenol resin secondly. The method comprises the following steps: mixing fenol, 138.4 phosphoric acid and water according to the proportion; dropping the extractant of formaldehyde and methyl isobutyl ketone with uniform speed; washing the product with distilled water; getting white solid state bisphenol F by vacuum dehydration; adding formaldehyde, oxalic acid, alcaine and water in bisphenol F and heating until boiling; stopping the reaction after keeping the temperature; aspirating the upper layer acid liquor; washing with distilled water; proceeding with vacuum dehydration; getting the linear bisphenol F formaldehyde-phenol resin. The invention avoids the roofing copper system property step-down problem of high free phenol in linear bisphenol F formaldehyde-phenol resin, which avoids the bad shockproof property problem of the roofing copper system in linear bisphenol F formaldehyde-phenol resin.

Description

technical field [0001] The invention relates to a novolac bisphenol F phenolic resin and a preparation method thereof. Background technique [0002] At present, with the rapid development of electrical and electronic fields and their composite materials, the demand for copper clad laminates is increasing, and the performance requirements for cured epoxy resins are also getting higher and higher. The new curing agent-phenolic resin in the epoxy resin system for copper clad laminates developed in the late 1980s has become an important aspect to promote the development of copper clad laminates technology. The high-density benzene ring structure in the phenolic resin molecule increases the rigidity of the molecule, and the numerous hydroxyl groups in the molecule can cause the epoxy group in the epoxy resin molecule to undergo a ring-opening reaction to increase the cross-linking density of the cured product, thereby improving the epoxy curing effect. The glass transition tempe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/20
Inventor 陈立新
Owner NORTHWESTERN POLYTECHNICAL UNIV
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