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pH-responsive amino sodium lignosulphonate as well as preparation method and application thereof

A sodium lignosulfonate, amine-based technology, applied in botanical equipment and methods, applications, animal repellents, etc., can solve problems such as pH responsiveness that is not involved, and achieve widening product added value, widening applications, The effect of broadening the application field

Inactive Publication Date: 2015-10-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, most of the amination reactions of lignin use alkali lignin as raw material, and there are few reports on the amination reaction of lignosulfonate, and none of them involve its pH responsiveness.

Method used

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  • pH-responsive amino sodium lignosulphonate as well as preparation method and application thereof
  • pH-responsive amino sodium lignosulphonate as well as preparation method and application thereof
  • pH-responsive amino sodium lignosulphonate as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Dissolve 100g of sodium lignosulfonate in 400g of water, adjust the pH to 12, activate in a water bath at 50°C for 0.5h, add 50g of diethylenetriamine, slowly add 50g of formaldehyde dropwise, and complete the dropwise addition within 0.5h. Raise the temperature to 70°C and continue the reaction for 4 hours to obtain a sodium lignosulfonate solution;

[0042] (2) Extract the sodium amine lignosulfonate solution with 100 mL of ethanol, then wash and filter with 300 mL of petroleum ether, and freeze-dry to obtain powdered sodium amine lignin sulfonate.

[0043] figure 1 It is the hydrogen nuclear magnetic spectrum of sodium lignosulfonate and sodium amine lignosulfonate. It can be clearly seen from the figure that compared with sodium lignosulfonate, sodium amine lignosulfonate weakens the aromatic proton peak at a chemical shift of 6.50-7.50ppm, and that at 2.50~3.00ppm is connected to the N element. The alkyl proton peak is significantly enhanced. This shows that the a...

Embodiment 2

[0057] (1) Dissolve 100g of sodium lignosulfonate in 150g of water, adjust the pH to 10, activate it in a 60℃ water bath for 1.0h, add 20g of triethylamine, slowly add 20g of acetaldehyde dropwise, finish the dropwise addition within 1h, and increase the temperature. To 80°C, continue to react for 2h to obtain sodium lignosulfonate solution;

[0058] (2) Extract the sodium amine lignosulfonate solution with 200 mL of methanol, wash and filter with 200 mL of petroleum ether, and freeze-dry to obtain powdered sodium amine lignin sulfonate.

Embodiment 3

[0060] (1) Dissolve 100g of sodium lignosulfonate in 200g of water, adjust the pH to 11, activate it in a 70℃ water bath for 1.0h, add 200g of diethylamine, slowly add 200g of propionaldehyde dropwise, the addition is complete within 1h, and the temperature rise To 90℃, continue to react for 3h to obtain sodium lignosulfonate solution;

[0061] (2) Extract the sodium amine lignosulfonate solution with 300 mL of propanol, wash and filter with 200 mL of petroleum ether, and freeze-dry to obtain powdered sodium amine lignin sulfonate.

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Abstract

The invention discloses a preparation method and application of pH-responsive amino sodium lignosulphonate. The preparation method comprises the following steps: dissolving sodium lignosulphonate in water to prepare a sodium lignosulphonate water solution, regulating the pH of the solution to be 10-13, and activating at 50-70 DEG C for 0.5-1.0 hour; adding an amination modifier, dropwise adding an aldehyde reagent, and reacting at 70-90 DEG C for 2-4 hours after the dropwise adding, so as to obtain an amino sodium lignosulphonate water solution; extracting the obtained amino sodium lignosulphonate water solution by virtue of an alcohol reagent, washing residual solids by virtue of petroleum ether after the extraction, and carrying out freeze drying on washed remnants. The amino sodium lignosulphonate prepared by virtue of the preparation method has remarkable pH response characteristic; by regulating the pH of the water solution of the product, the molecular configuration and the aggregation extent of the product can be changed, and a regular nanoparticle structure can be spontaneously formed; the amino sodium lignosulphonate can be used as a wall material to be applied field of pesticide microcapsules and is hopefully applied to the field of lignin-based nanometer materials.

Description

Technical field [0001] The invention relates to a preparation method of pH-responsive sodium lignosulfonate and its use as a wall material to prepare pesticide microcapsules. Specifically speaking, it uses sodium lignosulfonate as a byproduct of wood pulp or bamboo pulp sulfite pulping as raw materials, and performs Mannich reaction with polyamines and aldehydes in alkaline aqueous solution to prepare a pH-responsive amine Sodium lignosulfonate. Background technique [0002] Lignin is the second largest natural renewable resource in nature and an important resource for mankind in the future. Most of the industrial lignin raw materials come from the paper industry. So far, more than 95% of domestic lignin is directly discharged into rivers in the form of "black liquor" or burned after being concentrated, and is rarely effectively used. As a kind of abundant and renewable biological resources, lignin has gradually aroused people's widespread concern, especially when non-renewabl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00A01N25/28A01N43/90
Inventor 邱学青周明松许锐林杨东杰邓永红
Owner SOUTH CHINA UNIV OF TECH
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