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Preparation method of acidic ionic liquid resorcinol formaldehyde resin copolymer material

The technology of resorcinol formaldehyde resin and acid ionic liquid is applied in the field of preparation of acid ionic liquid resorcinol formaldehyde resin copolymer material, which can solve the problems of difficult stratification and inability to recover, and achieves easy recovery and good catalytic effect. , the effect of high catalytic activity

Inactive Publication Date: 2012-08-08
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the recovery of ionic liquids during use, especially after reacting with polar alcohols and carboxylic acids, cannot be recovered because they will be dissolved in organic matter and difficult to separate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] The preparation of the 1st step, ylide:

[0031] Weigh 4-vinylpyridine and propanesultone according to the ratio of the amount of substances to 1:1, and stir at room temperature for 72 hours to obtain a solid salt, then filter it with ether or ethyl acetate with a mass concentration greater than 99%. After the ester was washed 3 times, vacuum drying was carried out at 60°C to obtain the ylide;

[0032] Step 2, Acidification:

[0033] Dissolve the ylide in ethanol (1 gram of solid to 5 grams of ethanol), add sulfuric acid, the amount of sulfuric acid is equal to the amount of the ylide, and stir and mix at room temperature for 4 hours to obtain the corresponding anion as hydrogen sulfate The ionic liquid solution of the root is subjected to vacuum distillation at 50° C. to remove the solvent ethanol to obtain the ionic liquid monomer;

[0034] The 3rd step, the synthesis of ionic liquid polymer:

[0035] Dissolve the ionic liquid monomer in water, the amount of water ...

Embodiment 2-4

[0039] The preparation method is the same as in Example 1, the difference is that different pyridine compounds are used, and the properties of the acidic ionic liquid resorcinol-formaldehyde resin copolymer material prepared by it are shown in Table 1.

[0040] Table 1: Properties of acidic ionic liquid resorcinol-formaldehyde resin copolymer materials prepared by different pyridine compounds.

[0041] Example pyridine Acid value / mmol / g Thermal decomposition temperature / ℃ 2 3-vinylpyridine 4.5 218 3 2-vinylpyridine 4.4 216 4 4-allylpyridine 4.3 210

[0042] .

Embodiment 5-7

[0044] The preparation method is the same as in Example 1, except that the properties of the acidic ionic liquid resorcinol-formaldehyde resin copolymer material prepared by adjusting the ratio of resorcinol to ionic liquid monomer are shown in Table 2.

[0045] Table 2: Properties of acidic ionic liquid resorcinol-formaldehyde resin copolymer materials prepared with different ratios of resorcinol and ionic liquid monomers.

[0046] Example n(ionic liquid monomer) / n(resorcinol) Acid value / mmol / g Thermal decomposition temperature / ℃ 5 1：0.5 5.6 208 6 1：1.2 4.3 221 7 1:1.5 4.0 225

[0047] .

[0048] 2. Application examples.

[0049] The acidic ionic liquid resorcinol-formaldehyde resin copolymer material prepared in Example 1 was used to catalyze esterification reaction, condensation reaction, alkylation reaction and etherification reaction to obtain the following examples.

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Abstract

The invention discloses a preparation method of an acidic ionic liquid resorcinol formaldehyde resin copolymer material, and belongs to the technical field of organic chemical synthesis. The method is characterized by comprising the steps of: reacting vinyl pyridine compound with sultone to obtain ethylenic bond-containing sulfonic ylid; acidulating by sulfuric acid to obtain sulfonic functionalized ionic liquid monomer with anion of acid radical; carrying out self-assembly on the ionic liquid monomer to form an ionic liquid polymer solution; and then adding resorcinol and formaldehyde in theionic liquid oligomer solution; condensing at 65-95 DEG C for 60-120 hours; carrying out rotary evaporation to dryness; and placing at 180-300 DEG C for condensation reaction for 2-32 hours to obtainthe acidic ionic liquid resorcinol formaldehyde resin copolymer material. The material synthesized by the method of the invention has advantages of high thermal stability, high acid value and good catalytic effect.

Description

Technical field: [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing an acidic ionic liquid resorcinol-formaldehyde resin copolymer material. 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 by removing the salt generated by neutralization. However, a considerable amount of ene...

Claims

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Application Information

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IPC IPC(8): C08G8/22B01J31/06C07C69/704C07C67/08C07C39/08C07C37/16C07C43/20C07C41/09C07D317/72
Inventor 梁学正
Owner SHAOXING UNIVERSITY
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