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A sulfonated cellulose water reducer based on a porous carbon sulfonic acid catalyst loaded with elemental tin and its preparation method

A technology of carbon sulfonic acid and elemental tin, which is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve rare problems, reduce severity, improve catalytic activity, and improve use performance effect

Active Publication Date: 2021-01-19
浙江工业大学上虞研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be known from the above prior art that sulfonated cellulose water reducers with different degrees of sulfonation can be prepared by using cellulose with different crystallinity as raw materials and through the action of different sulfonating agents. There are few studies on cellulose superplasticizers

Method used

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  • A sulfonated cellulose water reducer based on a porous carbon sulfonic acid catalyst loaded with elemental tin and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) According to the mass ratio of carbon source and silicon dioxide of 2:1, immerse the nano-silica microspheres in the sucrose solution, stir evenly at room temperature, heat up to 90°C to remove the solvent, and pass in an inert gas, Raise the temperature to 170°C at a rate of 3°C / min, keep warm for pre-carbonization for 3 hours, then raise the temperature at a rate of 1°C / min to 420°C, keep warm and carbonize for 2 hours, take it out, and use hydrofluoric acid and nitric acid with a volume ratio of 95:2 The mixture was desiliconized, ground and dried to obtain a porous carbon support.

[0029] (2) According to the molar ratio of sulfur trioxide to porous carbon carrier is 1:1, add porous carbon carrier to a mixture containing 5.2% sulfur trioxide and air as a sulfonating agent, heat up to 35°C for sulfonation, and the sulfonating agent The residence time is 0.1s, dilute and filter to obtain a porous carbon sulfonic acid carrier.

[0030] (3) According to the molar ...

Embodiment 2

[0033] (1) According to the mass ratio of carbon source and silicon dioxide of 2.2:1, immerse the nano-silica microspheres in the glucose solution, stir evenly at room temperature, heat up to 100°C to remove the solvent, and pass in an inert gas, Raise the temperature to 180°C at a rate of 5°C / min, heat-preserve and pre-carbonize for 4 hours, then raise the temperature to 480°C at a rate of 2°C / min, heat-preserve and carbonize for 4 hours, take it out, and use hydrofluoric acid and nitric acid with a volume ratio of 98:5 The mixture was desiliconized, ground and dried to obtain a porous carbon support.

[0034] (2) According to the molar ratio of sulfur trioxide to porous carbon carrier is 1.03:1, add porous carbon carrier to a mixture containing 5.6% sulfur trioxide and air as a sulfonating agent, heat up to 42°C for sulfonation, and the sulfonating agent The residence time is 0.15s, dilute and filter to obtain a porous carbon sulfonic acid carrier.

[0035] (3) According to t...

Embodiment 3

[0038] (1) According to the mass ratio of carbon source to silicon dioxide of 2.1:1, the nano-silica microspheres were immersed in sucrose, glucose and starch solution, stirred evenly at room temperature, and then heated to 95°C to remove the solvent, and Inject inert gas, heat up to 175°C at a rate of 3.5°C / min, hold for 3.5 hours for pre-carbonization, then heat up to 450°C at a rate of 1.3°C / min, hold for 2 hours for carbonization, take it out, and use hydrogen with a volume ratio of 96:3 The mixture of hydrofluoric acid and nitric acid removes silicon, grinds and dries to obtain a porous carbon support.

[0039] (2) According to the molar ratio of sulfur trioxide and porous carbon carrier of 1.01:1, the porous carbon carrier is added to a mixture containing 5.5% sulfur trioxide and air as a sulfonating agent, and the temperature is raised to 38°C for sulfonation, and the sulfonating agent The residence time is 0.13s, dilute and filter to obtain a porous carbon sulfonic aci...

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Abstract

The invention provides a sulfonated cellulose water reducer based on a porous carbon sulfonic acid catalyst loaded with elemental tin, and a preparation method of the sulfonated cellulose water reducer. The preparation method comprises the following steps: mixing nano-silica microspheres with a carbon source solution, carrying out heating to remove the solvent, carrying out heating for carbonizing, and removing silicon to obtain a porous carbon carrier; then carrying out heating sulfonation treatment on the porous carbon carrier to obtain a porous carbon sulfonic acid carrier; placing the porous carbon sulfonic acid carrier in a tin dichloride solution and a ferric iron solution in sequence, maintaining the system to be acidic, and carrying out reacting, spin-drying and high-temperature calcination to obtain the porous carbon sulfonic acid catalyst loaded with elemental tin; and finally, putting dichloromethane containing activated micro-nano cellulose slurry into an intermittent reaction kettle, adding the porous carbon sulfonic acid catalyst loaded with elemental tin, carrying out pre-sulfonation treatment under rapid stirring and fast heating, then introducing a sulfonating agent, carrying out a heat-preservation reaction under high-speed stirring and slow heating, and rapidly carrying out cooling to room temperature after the reaction is stopped to obtain the sulfonated cellulose water reducer based on the porous carbon sulfonic acid catalyst loaded with elemental tin.

Description

technical field [0001] The invention belongs to the technical field of sulfonated water reducer materials, and in particular relates to a sulfonated cellulose water reducer based on a porous carbon sulfonic acid catalyst loaded with elemental tin and a preparation method thereof. Background technique [0002] Cellulose is a linear macromolecule formed by connecting many D-glucopyranose with β-(1-4) glycosidic bonds. There are a large number of hydroxyl groups on the cellulose molecular chain, which is easy to undergo chemical reactions and easy to modify and utilize. and other characteristics, the ionic groups that can interact with the surface of the material can be introduced into the cellulose molecular chain to prepare a sulfonated cellulose water reducer. Sulfonation reaction is a reaction process of introducing sulfonic acid groups or sulfonyl chloride groups into organic molecules. The sulfonation reaction can be divided into direct sulfonation and indirect sulfonatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B24/38B01J27/02C04B103/30
CPCB01J27/02C04B40/0039C04B2103/302C04B24/383C04B14/06C04B14/022C04B22/06C04B22/04C04B24/005
Inventor 许萌叶青罗书平
Owner 浙江工业大学上虞研究院有限公司