Composite catalytic membrane applied to catalytic esterification and preparation method thereof

A technology for catalyzing esterification and catalytic membrane, which is applied in catalyst activation/preparation, reaction preparation of ester group and hydroxyl group, preparation of organic compounds, etc. and other problems, to achieve the effect of high catalytic esterification efficiency, easy control, and improved catalytic performance

Inactive Publication Date: 2014-07-02
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after the large particle catalyst was reused 3 times, the conversion rate dropped to 89%.
Chinese patent CN101045688 (2007) reported a new type of esterification reaction device, that is, the lactic acid was added to the reaction system containing alcohol and catalyst to react through the porous membrane, and then combined with the pervaporation membrane to remove the lactic acid in the reaction system in time. Water, under the given conditions, the yield of methyl lactate reaches more than 96%, but the catalyst is directly added to the reaction system, which not only makes it difficult to reuse the catalyst, but even pollutes the product.
[0006] Although polymer / solid catalyst hybrid catalytic membranes can be prepared by hybridizing polymers and solid catalysts and exhibit better catalytic efficiency and longer service life, the catalytic membranes prepared by this method are generally dense structures. The solid catalyst on the surface of the membrane can play a catalytic role, but the catalyst on the membrane body is difficult to play a catalytic role, and there are defects in the specific surface area of ​​the catalytic membrane and the low efficiency of the catalyst.

Method used

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  • Composite catalytic membrane applied to catalytic esterification and preparation method thereof
  • Composite catalytic membrane applied to catalytic esterification and preparation method thereof
  • Composite catalytic membrane applied to catalytic esterification and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The non-woven fabric was modified by alkali-catalyzed hydrolysis, as follows: 5 g / L NaOH ethanol solution and 1 g / L cetyltrimethylammonium bromide aqueous solution were prepared respectively. Put the non-woven fabric into a three-neck flask, 50 mL NaOH ethanol solution, 1 mL immobilization accelerator, and then heat it in a constant temperature water bath at 40°C for 1 h, take it out, and soak it in ethanol for 2 h to remove unreacted reagents. Then the samples were dried for 3 hours in an electric constant temperature blast drying oven. The specific surface area and porosity of the basement membrane were measured by mercury porosimetry. The performance is shown in Table 1:

[0032] Table 1 Determination of performance parameters of different base films

[0033]

[0034] Then, the sulfated polyvinyl alcohol (4% sulfonation degree) was made into a 1 wt% casting solution with distilled water as a solvent, and then the solid acid zirconium sulfate Zr(SO 4 ) 2 Add, ...

Embodiment 2

[0037] The basement membrane modification method and casting solution preparation are the same as in Example 1. The difference is that the surface coating method is used to make the film: put the clean and dry glass plate on the pre-leveled scraping film platform, fix the non-woven fabric on the scraping film plate, and ensure that the non-woven fabric is flat and wrinkle-free and Fix it, pour a certain amount of casting solution evenly on one end of the non-woven fabric, scrape it into a uniform film of a certain thickness with a glass rod, then stay in the air for one minute, put it into an ethanol coagulation bath, and after solidification for 60 minutes, Add a cross-linking solution (50% glutaraldehyde aqueous solution and absolute ethanol at a volume ratio of 1:30) and soak for 2 hours for cross-linking to obtain a porous composite catalytic membrane. The catalytic test conditions are as in Example 1, and the catalytic properties of the composite membranes obtained by dif...

Embodiment 3

[0041] Preparation of composite membranes by dipping method is as described in Example 1, except that the sulfonated polymer (select polyvinyl alcohol, polyethylene-vinyl alcohol, polyvinylidene fluoride, polyacrylonitrile, various cellulose, polysulfone or one of the polyethersulfone polymers, the degree of sulfonation is 4%), and N, N-dimethylpyrrolidone is used as a solvent to prepare a 5 wt% casting solution. The corresponding sulfonated polymer / solid acid porous composite catalytic membrane can be obtained. At a temperature of 65°C, the mass ratio of oleic acid to methanol is 1:3, and the molar ratio of acetic acid to ethanol is 1:3. The catalytic esterification performance of the porous composite catalytic membrane with cloth as the base membrane is shown in Table 3.

[0042] Table 3 Effect of different sulfonated polymers on catalytic esterification performance

[0043]

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Abstract

Provided are a composite catalytic membrane for catalyzing an esterification reaction and a preparation method thereof. The composite catalytic membrane has a porous structure, with non-woven fabric as the base film, and a catalytic coating is compounded on the surface of the non-woven fabric and in the pores and gaps of the non-woven fabric fibers. The catalytic coating uses a solid acid as a catalyst to polymerize Compound or modified sulfonated polymer is used as film-forming material, and the film is formed by coating method or impregnation method, and after forming, it is cross-linked to obtain a composite catalytic membrane. Utilizing the microporous structure and developed specific surface of the composite catalytic membrane, the catalytic esterification and the greening and high efficiency of the biodiesel preparation process are realized. The composite catalytic membrane has high mechanical strength and good repetition stability, and is easy to realize the continuous production repetition of the catalytic esterification process. The preparation process is simple and easy to control and scale up.

Description

technical field [0001] The invention belongs to the technical field of membrane materials and catalysis, and in particular relates to a composite catalytic membrane for catalyzing esterification and a preparation method thereof, in particular to a novel composite membrane which can be used for catalytic esterification of organic acids and alcohols and preparation of biodiesel. Catalytic membrane and method for its preparation. The international patent main classification number is proposed to be Int.Cl.B01D71 / 02. Background technique [0002] Organic carboxylic acid esters are important fine chemical products, often used as solvents and fragrances, and can be used in synthetic fragrances, cosmetics, food and feed additives, surfactants, anti-corrosion and anti-fungal agents, plasticizers for rubber and plastics, and pharmaceuticals. Raw materials and intermediates, etc., long-chain organic carboxylic acid esters are also used as biodiesel to replace petrochemical diesel. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01J31/26B01D67/00B01D69/12B01J35/10
CPCB01J27/053C10G2400/04B01D69/02B01D2325/10B01J31/06Y02E50/13B01J37/02C11C3/04C11C3/003B01D2325/24C07C67/03C10L1/026B01J35/065C07C67/08B01J27/19B01D71/82B01D69/145B01D69/148B01D2325/28Y02E50/10C07C69/52C07C69/14
Inventor 李建新何本桥石文英程煜
Owner TIANJIN POLYTECHNIC UNIV
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