Preparation method of sulfoacid-type cation exchange resin catalyst

A cation exchange and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, fatty acid esterification, etc., can solve the problems of complex process, expensive, strong corrosion, etc., and achieve efficient catalytic esterification reaction , simple preparation process and high thermal stability

Inactive Publication Date: 2014-03-19
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction has the following disadvantages: concentrated sulfuric acid cannot be recovered from the product, subsequent treatment is difficult, and the problem of environmental pollution is increased; in addition, concentrated sulfuric acid is very corrosive to equipment, which inevitably increases the cost of equipment and materials.
The implementation of this technical idea has the following three technical routes: first, use the aromatic monomer whose core is halogenated to copolymerize with the crosslinking agent divinylbenzene, and then undergo sulfonation, as described in JP73-8675 and GB1393594. Disadvantage is that halogenated monomers are rare and expensive; two, the method for carrying out halogenation modification to the aromatic nucleus of sulfonic acid resin, as described in US3256250, has a shortcoming of poor thermal stability of catalyst active mass; three, adopts Aromatic series cation exchange resins are first halogenated and then sulfonated as the preparation method of high thermal stability cation exchange resin catalyst disclosed in CN1167011A. This method has less three wastes and low cost, but the whole technological process is more complicated

Method used

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  • Preparation method of sulfoacid-type cation exchange resin catalyst
  • Preparation method of sulfoacid-type cation exchange resin catalyst
  • Preparation method of sulfoacid-type cation exchange resin catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh 2.0 g of dry macroporous cross-linked polystyrene-divinylbenzene white balls into a three-necked flask equipped with a stirring and reflux condenser, add 10.0 g of dichloroethane, and swell at 20°C for 2 hours. Add 20.0 g of methanesulfonic acid, and start stirring at a slow speed. Raise the temperature to 85°C and keep it warm for 6.0h; raise the temperature to 100°C and keep it warm for 3.0h to remove dichloroethane by distillation. Cool to room temperature, add 40% methanesulfonic acid to wash, then slowly add deionized water dropwise under stirring, repeatedly wash until neutral, and vacuum dry at 60-120°C to obtain a macroporous sulfonic acid cation exchange resin catalyst.

[0013] Calculate the exchange capacity of the catalyst:

[0014]

[0015] in:

[0016] M—concentration of NaOH standard solution (mol / L);

[0017] V—the volume of NaOH standard solution used for titration (mL);

[0018] W—weight of dry resin (g).

[0019] Hydrothermal stability t...

Embodiment 2

[0028] Weigh 2.0 g of dry macroporous cross-linked polystyrene-divinylbenzene white balls, add 4.5 g of dichloroethane, and heat up to 45° C. to swell for 3.0 h. Add 10.0 g of methanesulfonic acid, and start stirring at a slow speed. Raise the temperature to 95°C and keep it warm for 3.0h; raise the temperature to 120°C and keep it warm for 2.0h to remove dichloroethane by distillation. Cool to room temperature, add 80% methanesulfonic acid to wash, then slowly add deionized water dropwise under stirring, repeatedly wash until neutral, and vacuum dry at 60-120°C to obtain a macroporous sulfonic acid cation exchange resin catalyst.

[0029] The exchange capacity of the obtained catalyst and the conversion rate of FFA when used in the esterification reaction are shown in Table 1.

Embodiment 3

[0033] Weigh 2.0 g of dry macroporous cross-linked polystyrene-divinyl benzene white balls into a three-necked flask equipped with a stirring and reflux condenser, add 1.0 g of dichloroethane, and heat up to 80°C to swell for 10 min. Add 40.0 g of methanesulfonic acid, and start stirring at a slow speed. Raise the temperature to 70°C and keep it warm for 1.0h; raise the temperature to 150°C and keep it warm for 0.5h to remove dichloroethane by distillation. Cool to room temperature, add diluted 70% methanesulfonic acid to wash, then slowly add deionized water dropwise under stirring, wash repeatedly until neutral, and vacuum dry at 60-120°C to obtain a macroporous sulfonic acid cation exchange resin catalyst .

[0034] Table 1 shows the exchange capacity of the catalyst and the conversion rate of FFA when used in the esterification reaction.

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Abstract

The invention discloses a preparation method of a sulfoacid-type cation exchange resin catalyst. The preparation method of the sulfoacid-type cation exchange resin catalyst comprises the following steps: swelling for 10 minites-3 hours at 20-80 DEG C by taking a macropore crosslinked polystyrene-divinylbenzene copolymer as a sulfonation carrier and taking dichloroethane as a solvent, reacting for 1.0-6.0 hours at 70-95 DEG C by taking methanesulfonic acid as a sulfonation reagent, warming up to 100-150 DEG C, and reacting for 0.5-3.0 hours; and then removing dichloroethane, washing, and drying to obtain a target product. The reaction time is short; the preparation process is simple; the exchange capacity of the obtained high-activity sulfoacid-type cation exchange resin catalyst is even greater than 5.5mg / g; the sulfoacid-type cation exchange resin catalyst can catalyze esterification reaction efficiently, can efficiently convert free fatty acid, is high in thermal stability, and is not affected by water generated in the esterification.

Description

Technical field: [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a preparation method of a sulfonic acid type cation exchange resin catalyst. Background technique: [0002] Biodiesel is a mixture of Fatty Acid Methyl Ester (FAME) produced by the transesterification of animal and vegetable oils with simple alcohols. It is a clean fuel that can replace petrochemical diesel. Compared with biodiesel, it has many advantages such as renewable, environment-friendly, convenient transportation and storage, and safety. At present, in China, low-cost high-acid value waste frying oil and non-edible oil are mainly used as raw materials. This kind of waste oil is large in volume, relatively pure, easy to collect and low in cost, and is the first-class raw material for biodiesel production. However, these non-edible oils contain a large amount of free fatty acids (Free Fatty Acid, FFA), and direct transesterification will cause s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10C11C3/10
Inventor 吕鹏梅刘莉梅袁振宏杨玲梅罗文李惠文苗长林王治元
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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