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A kind of preparation method of bisphenol F and three, tetracyclic phenolic resins

A phenolic resin, crude technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of high product cost, low yield, no large-scale production, etc., to reduce the use of solvents , reduce production cost, change the effect of phenol residue

Inactive Publication Date: 2011-12-14
SHANDONG LAIWU RUNDA NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few reports on the synthesis of bisphenol F in China. Although some institutions are still conducting research, there are still problems such as high phenol-formaldehyde ratio, low yield, and difficulty in direct recycling and reuse of resin contained in the catalyst, which makes energy consumption in the production process Large size, high product cost, complex product post-processing and other issues, there is no report of large-scale production in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of production method of bisphenol F and three, tetracyclic phenolic resin, is finished by following steps:

[0028] (1), take the phenol 1mol of 99.9% content used, 37% formaldehyde 0.1mol, hydroxyethylidene diphosphoric acid 28 grams, toluene 86ml, two parts of deionized water by the amount of substance, every part of deionized water 28 grams;

[0029] (2), the phenol measured, hydroxyethylidene diphosphoric acid and the first part of deionized water are mixed and stirred evenly in the reactor;

[0030] (3), heat up, when material temperature is at 40 ℃, add dropwise the aldehyde that takes, then at 40 ℃, insulation reaction 8 hours;

[0031] (4), after the reaction finishes, cool down to below 30 ℃, static layering;

[0032] (5), after separating the upper layer oil phase from the lower layer water phase, add a second portion of deionized water to the oil phase, and neutralize it to pH 3.5-4 with 25% sodium hydroxide solution, then statically separate the laye...

Embodiment 2

[0041] A kind of production method of bisphenol F and three, tetracyclic phenolic resin, is finished by following steps:

[0042] (1), get used 99.9% content phenol 1mol, 37% formaldehyde 0.1mol, hydroxyethylidene diphosphoric acid 28 grams, toluene 86ml, two parts of deionized water by the amount of substance, every part of 28 grams;

[0043](2), the phenol measured, hydroxyethylidene diphosphoric acid and the first part of deionized water are mixed and stirred evenly in the reactor;

[0044] (3), heating up, when material temperature is at 50 ℃, dropwise add the formaldehyde that takes, then at 50 ℃, insulation reaction 8 hours;

[0045] (4), after the reaction finishes, cool down to below 30 ℃, static layering;

[0046] (5), after separating the upper layer oil phase from the lower layer water phase, add a second portion of deionized water to the oil phase, and neutralize it to pH 3.5-4 with 25% sodium hydroxide solution, then statically separate the layers;

[0047] (6),...

Embodiment 3

[0055] A kind of production method of bisphenol F and three, tetracyclic phenolic resin, is finished by following steps:

[0056] (1), take the phenol 1mol of used 99.9% content, 37% formaldehyde 0.5mol and 56 grams of hydroxyethylidene diphosphoric acid by the amount of substance;

[0057] (2), the phenol that takes, hydroxy ethylidene diphosphoric acid and the formaldehyde that take are mixed and stirred in reactor;

[0058] (3), heating up, when material temperature is at 40 ℃, insulation reaction is 8 hours;

[0059] (4), after the end of the reaction, cool down to below 30°C and stand still;

[0060] (6), suction filtration after a large amount of crystals appear;

[0061] (7), after repeatedly washing with deionized water three times during the suction filtration process, place the mixture of crude bisphenol F and tricyclic and tetracyclic phenolic resins on the suspended filter cloth, and bake and dry in an oven at 50°C;

[0062] (8), the upper material of the filter...

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Abstract

The invention discloses a preparation method of bisphenol F and three- and four-ring phenolic resins, which is characterized in that it comprises the following steps: measuring phenol, formaldehyde and organic phosphoric acid catalyst; adding phenol, formaldehyde and organic phosphoric acid catalyst in sequence In the reaction kettle, the temperature is raised; after the reaction is completed, a large amount of crystals are precipitated after cooling down, suction filtered, and washed with water to obtain a mixture of crude bisphenol F and tricyclic and tetracyclic phenolic resins; place it on a suspended filter cloth, and in the oven Baking and drying, the obtained upper material of the filter cloth is crude bisphenol F, and the material filtered out of the filter cloth is tricyclic and tetracyclic phenolic resins; the filtered water phase is treated. The present invention adopts organophosphoric acid catalyst, can directly form crude bisphenol F without the step of solvent crystallization, greatly reduces the amount of solvent used, and reduces the complexity of later work; The tricyclic and tetracyclic phenolic resins produced by the reaction.

Description

technical field [0001] The invention relates to a preparation method of phenolic resin, which belongs to the technical field of chemical industry, and specifically relates to a preparation method of bisphenol F and three- and four-ring phenolic resins. The obtained bisphenol F and three- and four-ring phenolic resins are mainly used It is used in the production of bisphenol F epoxy resin, phenolic epoxy resin and polycarbonate, and can be used as a curing agent for epoxy resin, a modifier and stabilizer for phenolic resin. Background technique [0002] Bisphenol F is a new type of chemical raw material developed since the 1980s, mainly composed of three isomers of dihydroxydiphenylmethane. It is mainly used as low-viscosity epoxy resin, special polyester raw material and information recording paper additive, etc., and can be used as a raw material for polycarbonate. The epoxy resin made from bisphenol F is better than bisphenol A epoxy resin in viscosity, impact strength an...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20C08G8/10
Inventor 吕虎李长彬董小强吕华乐碧兰侯振兴张锋
Owner SHANDONG LAIWU RUNDA NEW MATERIAL
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