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Phenolic resin based solid acid, preparation method and application thereof

A technology of phenolic resin and solid acid, which is applied in the dehydration of hydroxyl-containing compounds to prepare ethers, the reaction preparation of carboxylic acids/symmetric anhydrides and saturated hydrocarbons, and the preparation of ethers. It can solve unsatisfactory problems and achieve high thermal stability and high catalytic performance. The effect of activity and large specific surface area

Inactive Publication Date: 2011-07-20
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In addition, in the inorganic system, zirconia (ZrO 2 ) is treated with sulfuric acid, and the obtained sulfuric acid trace (sulfuric acid trace) zirconia is a solid acid catalyst with the strongest acidity, but there are not many traces of sulfuric acid on the surface, and the number of acid points per unit weight is higher than that of liquid acid Much less, so far from meeting the above requirements

Method used

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  • Phenolic resin based solid acid, preparation method and application thereof
  • Phenolic resin based solid acid, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Synthesis of phenolic resin-based solid acid:

[0024] The first step, the synthesis reaction of carbon-based solid acid: PF phenolic resin and isethionic acid are stirred and mixed evenly in the ratio of 1:1 by mass, then placed in a quartz tube muffle furnace, and replaced by nitrogen gas The air was heated to 200°C in a nitrogen atmosphere for carbonization reaction for 12 hours to obtain a black solid;

[0025] Step 2, water washing, suction filtration and drying: After the solid is cooled to room temperature, add hot water above 80°C for washing, and filter until the filtrate is clear and acidic, and then put the solid in an oven at 120°C Drying was carried out for 1 day, and the acid value of the obtained catalyst was 1.3 mmol / g, and the thermal decomposition temperature was 160°C;

Embodiment 2-4

[0027] The preparation method is the same as in Example 1, the difference is that the carbonization condensation reaction time is adjusted, and the influence results of different reaction times are shown in Table 1.

[0028] Table 1: Different carbonation condensation reaction times and their results

[0029] Example

Embodiment 5-7

[0031] The preparation method is the same as that in Example 1, the difference is that the dosage of isethionic acid is adjusted, and the influence results of different dosages of isethionic acid are shown in Table 2.

[0032] Table 2. The amount of different isethionic acids and their results

[0033]

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Abstract

The invention discloses a phenolic resin based solid acid, a preparation method and application thereof, belonging to the technical field of chemical synthesis. The preparation method is characterized by comprising the steps of: with phenolic resin as a raw material and isethionic acid with a mass ratio of 1:0.5-1:2 with the raw material as an active molecule, undergoing a condensation reaction for 2-32h at a temperature of 180-300 DEG C, after the reaction is ended, adding hot water with the temperature of above 80 DEG C in the product for washing, filtering to remove free acidic matters, and then drying in a drying oven with the temperature of 120 DEG C to obtain the phenolic resin based solid acid. The phenolic resin based solid acid prepared in the invention has the advantages of highheat stability, high acid value, good catalytic activity, capability of being repeated in use, and the like.

Description

Technical field: [0001] The invention relates to a polar solvent-insoluble phenolic resin-based solid acid obtained by carbonizing phenolic resin containing phenolic hydroxyl groups and isethionic acid under high-temperature nitrogen conditions, and the use of the solid acid as a solid acid catalyst. Background technique: [0002] In today's crisis of energy problems and environmental problems, it has become the goal of modern chemical industry to efficiently generate target products with a small amount of energy without producing unnecessary by-products. Acid catalysts are indispensable in the modern chemical industry and are widely used in the manufacture of various products such as pharmaceuticals, petrochemical products, and polymer products. However, most of the currently used liquid acid catalysts are hydrochloric acid and sulfuric acid. . The liquid catalyst used in the production process needs to be neutralized by alkali, and separated and recovered from the product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J37/08C07C69/704C07C67/035C07D317/72C07C39/08C07C37/16C07C43/20C07C41/09
Inventor 梁学正
Owner SHAOXING UNIVERSITY
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