Technique for preparing methoxyl aralkyl ether oligomers

A methoxy aralkyl ether and manufacturing technology, which is applied in the field of thermosetting resin manufacturing, can solve problems such as difficulty in realizing large-scale industrial production, and achieve excellent application effects, broad development and application prospects, and less by-products

Inactive Publication Date: 2008-05-28
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because the chlorine gas and catalyst used in the preparation process are highly corrosive and toxic, and the reaction is accompanied by the formation of highly corrosive hydrochloric acid and hypochlorous acid, it is difficult to achieve large-scale industrial production of this type of reaction.

Method used

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  • Technique for preparing methoxyl aralkyl ether oligomers
  • Technique for preparing methoxyl aralkyl ether oligomers
  • Technique for preparing methoxyl aralkyl ether oligomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 2000ml three-necked bottle, equipped with constant pressure funnel, mechanical stirring and condensing device. First put 420g (14mol) of formaldehyde into the three-necked bottle. Add 588g (6mol) of concentrated sulfuric acid into the separatory funnel, and drop it into the three-necked flask. After the dropwise addition, pour 212g (2.00mol) of m-xylene and 192g (6mol) of methanol into a three-necked flask, keep stirring, and raise the temperature of the water bath to 60-70°C. React for 1 hour. Afterwards, the temperature was raised to make the reaction temperature reach 78-80° C., and a reflux phenomenon occurred, and the reaction was carried out in this state for 6 hours. After the reaction was completed, the system was cooled to room temperature and separated into layers, and the liquid in the lower layer was removed. The collected upper liquid was washed with 10% Na 2 CO 3 Wash with aqueous solution, and then wash with hot water at 60-70°C until neutral. The r...

Embodiment 2

[0030] 2000ml three-necked bottle, equipped with constant pressure funnel, mechanical stirring and condensing device. First put 420g (12.23mol) of formaldehyde into the three-necked bottle. Add 176g (1.8mol) of concentrated sulfuric acid into the separatory funnel, and dropwise into the three-necked flask. After the dropwise addition, 340 g (2.00 mol) of diphenyl ether and 256 g (8 mol) of methanol were poured into a three-necked flask, stirred continuously, and the temperature of the water bath was raised to 60-70°C. React for 1 hour. Afterwards, the temperature was raised to make the reaction temperature reach 78-80° C., and a reflux phenomenon occurred, and the reaction was carried out in this state for 6 hours. After the reaction was completed, the system was cooled to room temperature and separated into layers, and the liquid in the lower layer was removed. The collected upper liquid was washed with 10% Na 2 CO 3 Wash with aqueous solution, and then wash with hot wat...

Embodiment 3

[0034] 2000ml three-necked bottle, equipped with constant pressure funnel, mechanical stirring and condensing device. First put 120g (4mol) of formaldehyde into the three-necked bottle. Add 78.4g (0.8mol) of concentrated sulfuric acid into the separatory funnel, and dropwise into the three-necked flask. After the dropwise addition is complete, pour 240g (2.00mol) of 1,2,3-trimethylbenzene, 1,2,4-trimethylbenzene, a mixture of mesitylene and 128g (4mol) of methanol into a three-necked flask and keep stirring , and raise the temperature of the water bath to 60-70°C. React for 1 hour. Afterwards, the temperature was raised to make the reaction temperature reach 78-80° C., and a reflux phenomenon occurred, and the reaction was carried out in this state for 6 hours. After the reaction was completed, the system was cooled to room temperature and separated into layers, and the liquid in the lower layer was removed. The collected upper liquid was washed with 10% Na 2 CO 3 Wash w...

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Abstract

The invention relates to the technical field of thermosetting resin manufacture, in particular to a manufacturing technique of methoxy aralkyl ether oligomer. The invention obtains polymer by using methanol and formaldehyde under the condition of acid catalyst with at least one aralkyl compound and through condensation polymerization. Compared with the prior art, the invention avoids the use of catalyst of strong corrosiveness and toxicity, with few byproducts and without released corrosive substance; in addition, the method of the invention uses raw materials of low cost and has the advantages of simple manufacturing technique, good application effect and is applicable to a plurality of modified phenol-formaldehyde resin with wide development and application prospect.

Description

technical field [0001] The invention relates to the technical field of manufacturing thermosetting resins, in particular to a manufacturing technology of methoxy aralkyl ether oligomers. Background technique [0002] British scientists have pointed out that xylene can undergo chlorination reaction with chlorine gas under light conditions, and the reaction is as follows: [0003] [0004] The reaction product is composed of various structures, accompanied by the formation of hydrochloric acid and hypochlorous acid. In 1932, Jacobson reported the method of preparing aralkyl polymers using Fridedl-Crafts as a catalyst and benzyl chloride as a raw material. After 1965, British scientists used this reaction mechanism to synthesize aralkyl polymers and aralkyl ether polymers with different molecular weights and different structural units. This kind of polymer has good thermal stability, the mechanical loss of the material is very little after 1000 hours of treatment at 250 ° ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/263C07C41/01
Inventor 焦扬声王家樑
Owner EAST CHINA UNIV OF SCI & TECH
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