Pyridine polymerized ionic liquid solid acid catalyst, and preparation method and application thereof

A technology for polymerizing ionic liquids and solid acid catalysts, which is applied in catalytic reactions, carboxylate preparations, chemical instruments and methods, etc. It can solve the problems of slow suction filtration, serious waste acid pollution, and high corrosion of equipment, and achieves convenient operation, The effect of good product color and high product yield

Pending Publication Date: 2021-12-31
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although the traditional catalysts used in industry, such as p-toluenesulfonic acid, have high catalytic activity, there are still many problems, such as serious waste acid pollution, complicated post-treatment process, and p-toluenesulfonic acid is highly corrosive to equipment.
Chinese patent literature (publication number: CN102826999A) discloses a kind of metal solid acid S 2 O / TiO e -La 2 o 3 or solid acid ZnO / SiO 2 Carry out the method for preparing neopentyl glycol oleate for catalyst esterification, although the yield reaches 92%, but the amount of catalyst added is very high 4wt.% and this kind of metal solid acid catalyst synthesis condition requirement is high, needs 300 ~ High temperature of 700°C
Chinese patent literature (publication number: CN101139288A) uses SO 4 2- / TiO 2 -SiO 2 A method for preparing ethyl linoleate from linoleic acid and absolute ethanol catalyzed by a composite solid superacid, the esterification rate can reach more than 95%, but the preparation process of this type of metal solid acid catalyst is complicated. It takes more than four times to filter one step and the oxide particles generated are very fine, which leads to slow suction filtration and wastes a lot of water resources

Method used

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  • Pyridine polymerized ionic liquid solid acid catalyst, and preparation method and application thereof
  • Pyridine polymerized ionic liquid solid acid catalyst, and preparation method and application thereof
  • Pyridine polymerized ionic liquid solid acid catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] This embodiment is the prepared polymerized 1-(4-sulfonic acid butyl)-2-vinylpyridine ionic liquid solid acid, and its specific synthesis steps are:

[0035] Under the condition of stirring at 30°C, equimolar 1,4-butane sultone and vinylpyridine were added, the reaction was completed for 4 hours, and washed twice with ethyl acetate to obtain an ionic liquid intermediate. Add an appropriate amount of distilled water to the prepared ionic liquid intermediate to dissolve, add equimolar concentrated sulfuric acid, heat up to 40° C. and stir for reaction. After 3 hours of reaction, remove water by rotary evaporation to obtain an ionic liquid monomer. The amount of initiator azobisisobutyronitrile added is 0.1wt.% of the mass of the added ionic liquid monomer. The rate is 96.7%.

[0036] The structural formula of the polymerized 1-(4-sulfonic acid butyl)-2-vinylpyridine ionic liquid is as follows:

[0037]

Embodiment 2

[0039] This embodiment is the prepared polymerized 1-(4-sulfonic acid butyl)-2-propenylpyridine ionic liquid solid acid, and its specific synthesis steps are:

[0040] Add equimolar 1,4-butane sultone and propenylpyridine under stirring condition at 30°C. After 5 hours of reaction, wash with ethyl acetate twice to obtain an ionic liquid intermediate. Add an appropriate amount of distilled water to the prepared ionic liquid intermediate to dissolve, add equimolar concentrated sulfuric acid, heat up to 40° C. and stir for reaction. After 3 hours of reaction, remove water by rotary evaporation to obtain an ionic liquid monomer. The amount of initiator azobisisobutyronitrile added is 0.2wt.% of the mass of the ionic liquid monomer added. The heating temperature is 65°C, the reaction time is 3h, and the water is removed by rotary evaporation to obtain the propylene-based polymerized ionic liquid, polymerized ionic liquid The yield was 97.2%.

[0041] The structural formula of the ...

Embodiment 3

[0044] This embodiment is the prepared polymerized 1-(4-sulfonic acid butyl)-2-butenylpyridine ionic liquid solid acid, and its specific synthesis steps are:

[0045]Add equimolar 1,4-butane sultone and butenylpyridine under stirring condition at 30°C. After 6 hours of reaction, wash with ethyl acetate three times to obtain an ionic liquid intermediate. Add an appropriate amount of distilled water to the prepared ionic liquid intermediate to dissolve, add equimolar concentrated sulfuric acid, heat up to 60° C. and stir for reaction. After 5 hours of reaction, remove water by rotary evaporation to obtain an ionic liquid monomer. The amount of initiator azobisisobutyronitrile added is 0.3wt.% of the mass of the added ionic liquid monomer. The liquid yield was 95.4%.

[0046] The structural formula of the polymerized 1-(4-sulfonic acid propyl group)-2-butenylpyridine ionic liquid is as follows:

[0047]

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Abstract

The invention belongs to a biological lubricating oil preparation technology, and particularly relates to a pyridine polymerized ionic liquid solid acid catalyst, and a preparation method and application thereof. In a reaction for synthesizing neopentyl glycol oleate, the addition amount of a catalyst is 0.1-0.6 wt.% of the total amount of neopentyl glycol and oleic acid, the addition amount of a water-carrying agent toluene is 5-15 wt.% of the total amount of neopentyl glycol and oleic acid, reflux dehydration is performed for 2-5 hours, and a crude product obtained by the reaction is subjected to water washing, rotary evaporation and adsorption to obtain the final product. The polymerized ionic solid acid catalyst in the reaction is prepared by firstly synthesizing an ionic monomer and then polymerizing the ionic liquid, and the catalyst is mild in generation condition, easy to prepare, good in catalytic activity, free of corrosion to equipment and simple in reaction post-treatment, and the product can be repeatedly used.

Description

technical field [0001] The invention belongs to the preparation technology of biological lubricating oil, and in particular relates to a pyridine polymerized ionic liquid solid acid catalyst and a preparation method and application thereof. Background technique [0002] Synthetic lubricating oils have good thermal stability, wide liquid range, high viscosity index and good frictional lubrication characteristics. Among all synthetic lubricating oils, polyol esters are the representatives (Zhang Wei, Liu Dongzhi. The development and status quo of synthetic ester lubricating oils [J]. Chemical Propellants and Polymer Materials, 1998 (05): 8-10.) . Neopentyl glycol oleate not only satisfies the above aspects, but also has good antioxidant properties, is non-toxic, has no peculiar smell, has good biodegradability, and has no impact on the environment. It is suitable for high-speed spinning oil, aviation engine lubricating oil, metal high-temperature processing oil and other fie...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01J31/06B01J31/02C07C67/08C07C69/58C08F126/06
CPCB01J31/063B01J31/0284B01J31/0285C07C67/08C08F126/06B01J2231/49C07C69/58Y02P20/584
Inventor李为民陆宇涵任庆功崔志建叶彤
OwnerCHANGZHOU UNIV