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Porous biomass acidic solid material, and preparation and application thereof

A technology of acidic solids and biomass, which is applied in the preparation of carboxylic acid esters, organic compounds, lignin derivatives, etc. It can solve the problems of limited application range, low material specific surface area, complex process, etc., and achieve rich sources of raw materials , simple preparation process and high operational safety

Inactive Publication Date: 2015-07-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the product is separated, it is necessary to recycle the organic phase such as dispersant and surfactant, which is a complicated process
In addition, the specific surface area of ​​the material prepared by this method is low, and the application range is limited

Method used

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  • Porous biomass acidic solid material, and preparation and application thereof
  • Porous biomass acidic solid material, and preparation and application thereof
  • Porous biomass acidic solid material, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 100g of magnesium lignosulfonate, make it into an aqueous solution with a mass concentration of 30%, add 75g of a mass fraction of 37% formaldehyde solution into a pressure-resistant polyester bottle, add 10g of SBA-15 as a template, mix, stir, and add to the reaction Mass fraction is 35g of hydrochloric acid of 37% in container, stirs until solution mixes, airtight, is placed in 100 ℃ of ovens and reacts 24h. Then dry the prepared black material at 110 ° C, grind, dry, grind, treat with hydrofluoric acid at room temperature for more than 12 hours to remove the template, and treat with 1M sulfuric acid for 2 hours to ensure that the magnesium ions are completely exchanged, and wash to no sulfate Ions, drying, that is, porous biomass acidic material. Neutralization titration, the acid content that obtains this material is shown in Table 1. Make the material N 2 Under the physical adsorption, the adsorption-desorption curve was obtained. The specific surface area...

Embodiment 2

[0032] Weigh 100g of sodium lignosulfonate, make it into an aqueous solution with a mass concentration of 30%, add 75g of a mass fraction of 37% formaldehyde solution into a pressure-resistant polyester bottle, add 10g of SBA-15 as a template, mix, stir, and add to the reaction Mass fraction is 35g of hydrochloric acid of 37% in container, stirs until solution mixes, airtight, is placed in 100 ℃ of ovens and reacts 24h. Then dry the prepared black material at 110°C, grind, dry, grind, treat with hydrofluoric acid at room temperature for more than 12 hours to remove the template, and treat with 1M sulfuric acid for 2 hours to ensure that the sodium ions are completely exchanged, and wash until there is no sulfate. Ions, drying, that is, porous biomass acidic material. Neutralization titration, the acid content that obtains this material is shown in Table 1. Make the material N 2 Under the physical adsorption, the adsorption-desorption curve was obtained. The specific surface...

Embodiment 3

[0034] Weigh 100g of sodium lignosulfonate, make it into an aqueous solution with a mass concentration of 30%, add 75g of a mass fraction of 37% formaldehyde solution into a pressure-resistant polyester bottle, add 100g of 30%wt silica sol with different particle sizes as a template, Mix and stir, and dropwise add 35 g of hydrochloric acid with a mass fraction of 37% to the reaction vessel, stir until the solution is uniformly mixed, airtight, and place in a 100° C. oven for reaction for 24 hours. Then dry the prepared black material at 110°C, grind, dry, grind, treat with hydrofluoric acid at room temperature for more than 12 hours to remove the template, and treat with 1M sulfuric acid for 2 hours to ensure that the sodium ions are completely exchanged, and wash until there is no sulfate. Ions, drying, that is, porous biomass acidic material. Neutralization titration, the acid content that obtains this material is shown in Table 1. Make the material N 2 Under the physical ...

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Abstract

The invention relates to a preparation method and application of a porous biomass acidic solid material. The preparation method is characterized by comprising the following steps: adding a lignosulfonate water solution having a certain concentration, an aldehyde compound, a template agent and a catalyst into a reaction vessel according to a certain ratio, uniformly mixing, and reacting at 50-220 DEG C for 2-120 hours; drying, grinding, removing the template, performing acid treatment, and washing to neutral; and drying to obtain the material. The porous material structurally contains multiple surface acidic groups such as sulfonic groups, carboxyl groups and hydroxyl groups, has a high surface distribution density and is a favorable porous acidic solid material. The material is used for esterification reaction, and the esterification yield is up to 85% or above. The material provided by the invention has the advantages of abundant raw material sources, controllable structure, simple preparation process and the like.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a preparation method and application of a porous biomass acidic solid material. Background technique [0002] Sulfonic acid-based solid materials have attracted attention as an acidic material that can replace liquid inorganic acids. The synthesis method of this kind of material mostly adopts the method of supporting sulfonic acid groups, mainly through incomplete carbonization of sulfonated compounds, or incomplete carbonization of organic substances and then sulfonation. [0003] CN10139668A sulfonates lignin in concentrated sulfuric acid at 50°C-95°C for several hours, and then carbonizes lignin under nitrogen protection at 300°C-450°C to prepare a lignosulfonate solid catalyst. CN102218342A uses biomass and aromatic compounds as substrates, reacts in a kettle at 150°C-220°C for 16-72 hours, grinds, washes, and sulfonates concentrated sulfuric acid to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00C07G1/00C08J9/26B01J31/06B01J31/02C07C67/08C07C69/14
CPCY02P20/584
Inventor 王峰张晓辰徐杰王业红陈贵夫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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