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Preparation method of modified lignin-sulfonate aliphatic water reducer

The technology of aliphatic water reducer and sulfonate, which is applied in the field of water reducer preparation, can solve the problems of long reaction time, small slump loss, and many raw materials used, so as to achieve cement with wide applicability and long-term durability. The effect of small loss and simple steps

Inactive Publication Date: 2018-11-06
王颖皓
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent (CN200910034276.0) a kind of aliphatic high-efficiency water reducer modified by lignosulfonate and its preparation method, acetone and formaldehyde are condensed, and then modified by lignosulfonate to obtain a small slump loss, The color of the water reducer is similar to that of concrete and the pollution is small. Because the water reducing rate and dispersion performance of the water reducer prepared by the method of sulfonation first and then grafting without oxidation are still not good enough, and the preparation time is long
Chinese patent (CN201110102226.9) is a preparation method of a polycarboxylic acid-based water reducer compound, which produces a water reducer with excellent performance, high water reducing rate, good dispersibility, and small slump loss, but the preparation method Complex, using many raw materials, long reaction time

Method used

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Examples

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Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of alkali lignin: at a temperature of 35°C, add malic acid and ammonia water to 100 parts of pulp black liquor to adjust the pH value to 12, raise the temperature to 65°C and add 6.5 parts of potassium dichromate and 0.6 manganese dioxide to react 1.5 h precipitation, the solution is centrifuged to obtain alkali lignin;

[0030] (2) Graft modification: first mix 80 parts of methyl ketone and 13 parts of p-aminosalicylic acid, then add 400 parts of water, alkali lignin prepared in step (1), and 39 parts of sodium 3-carboxybenzenesulfonate In the reaction vessel, adjust the pH of the reaction system to 11 with malic acid and ammonia water, stir evenly, and react at 40°C for 24 minutes; The modified alkali lignosulfonate aliphatic water reducer can be prepared by keeping it warm for 1 hour.

Embodiment 2

[0032] (1) Preparation of alkali lignin: at a temperature of 50°C, add salicylic acid and sodium hydroxide to 100 parts of pulp black liquor to adjust the pH value to 13, raise the temperature to 80°C and add 8 parts of hydrogen peroxide and 0.7 manganese dioxide to react 2.5 h precipitation, the solution is centrifuged to obtain alkali lignin;

[0033] (2) Graft modification: first mix 67 parts of acetone, 33 parts of pentanone and 18 parts of p-aminosalicylic acid, then mix 450 parts of water, alkali lignin prepared in step (1), and 47 parts of 3-carboxy Add sodium benzenesulfonate into the reaction vessel, control the pH of the reaction system to 12 with salicylic acid and sodium hydroxide, stir evenly, and react at 55°C for 28 minutes; After the addition is complete, keep the temperature at 100°C for 1.5 hours to prepare the modified alkali lignosulfonate aliphatic water reducer.

Embodiment 3

[0035] (1) Preparation of alkali lignin: at a temperature of 45°C, add sulfuric acid and potassium hydroxide to 100 parts of pulp black liquor to adjust the pH value to 14, raise the temperature to 75°C and add 9 parts of potassium permanganate and 0.4 parts of manganese dioxide to react 3h precipitation, the solution is centrifuged to obtain alkali lignin;

[0036] (2) Graft modification: first mix 115 parts of cyclohexanone and 16 parts of p-aminosalicylic acid, then mix 380 parts of water, alkali lignin prepared in step (1), and 40 parts of sodium 3-carboxybenzenesulfonate Add it into the reaction vessel, use sulfuric acid and potassium hydroxide to control and adjust the pH of the reaction system to 13, stir evenly, and react at 60°C for 26 minutes; then add 115 parts of formaldehyde and 185 parts of acetaldehyde dropwise at the same time, and add dropwise in 2 hours at a controlled rate After completion, keep the temperature at 90°C for 2 hours to prepare the modified alk...

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Abstract

The invention discloses a preparation method of a modified lignin-sulfonate aliphatic water reducer. The preparation method comprises the steps that certain pH and temperature of black liquor are controlled, and an oxidizing agent and a catalyst are added to prepare alkali lignin; a mixture of water, the alkali lignin, a ketone compound and p-aminosalicylic acid and 3-carboxyl sodium benzenesulfonate are added into a reaction container, a pH value is controlled, and then a aldehyde compound is added in a dropwise way to prepare the modified lignin-sulfonate aliphatic water reducer. The produced water reducer has the advantages of being low in water reducing rate, obvious in concrete reinforcement effect, small in slumping loss, good in dispersion adhesiveness, freezing resistance, seepageresistance and heat resistance, free of crystals at low temperature and not prone to steel bar corrosion when being used with concrete, the operation method is simple, the reaction time is short, andthe production efficiency is high.

Description

technical field [0001] The invention relates to a method for preparing a water reducer, in particular to a method for preparing a modified alkali lignosulfonate aliphatic water reducer. Background technique [0002] Water reducer is an admixture that reduces the amount of mixing water in the process of making concrete. After being added to concrete, it can disperse cement particles, reduce unit water consumption, and improve the fluidity of concrete; or it can reduce the unit amount of cement. Save cement. The water reducer components are divided into: lignosulfonate type water reducer, naphthalene type high-efficiency water reducer, melamine type high-efficiency water reducer, sulfamate type high-efficiency water reducer, fatty acid type high-efficiency water reducer Water agents, polycarboxylate-based superplasticizers. [0003] The preparation of lignosulfonate is convenient and simple, and the price is low, so it is widely used. Lignin exists in plants, and a large am...

Claims

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Application Information

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IPC IPC(8): C08G6/02C04B24/18C08H7/00C04B103/30
CPCC08G6/02C04B24/18C04B2103/302C08H6/00
Inventor 王颖皓
Owner 王颖皓
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