Preparation method and application of hydrophobic starch sulfate ester in cement water-reducing agent

A technology of starch sulfate and hydrophobization, which is applied in the field of chemistry and chemical engineering, to achieve the effect of widening the application range, low raw material cost and good water reducing effect

Active Publication Date: 2014-09-03
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of hydrophobized starch sulfate as a water reducing agent has not been reported

Method used

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  • Preparation method and application of hydrophobic starch sulfate ester in cement water-reducing agent
  • Preparation method and application of hydrophobic starch sulfate ester in cement water-reducing agent
  • Preparation method and application of hydrophobic starch sulfate ester in cement water-reducing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 19.4g of sulfamic acid and 2.4g of urea are fully ground and mixed, add 12.96g of dry cornstarch, mix evenly again, add a mixture of 2.5g of deionized water and 1.632g of benzyl alcohol, stir and mix evenly in a mixing cup, put Put it into an oven at 120° C. for 6 hours to obtain a crude product of benzyl hydrophobized starch sulfate. Add 50g of deionized water to the crude product to dissolve it, precipitate it with anhydrous methanol, wash it three times with 90% methanol aqueous solution, and dry the filter cake at 50°C for 4 hours to obtain a sulfonic acid group substitution degree of 0.71, a benzyl substitution degree of 0.04 benzyl hydrophobized starch sulfate.

Embodiment 2

[0020] 5.82g of sulfamic acid and 9.6g of urea are fully ground and mixed evenly, add 12.96g of dry cornstarch, mix evenly again, add a mixture of 3.0g deionized water and 0.816g benzyl alcohol, stir and mix evenly in a mixing cup, put Put it into an oven at 100° C. for 8 hours to obtain a crude product of benzyl hydrophobized starch sulfate. Add 50g of deionized water to the crude product to dissolve it, precipitate it with anhydrous methanol, wash it three times with 90% methanol aqueous solution, and dry the filter cake at 50°C for 4 hours to obtain a sulfonic acid group substitution degree of 0.25, benzyl substitution degree 0.03 benzyl hydrophobized starch sulfate.

Embodiment 3

[0022] 14.56g of sulfamic acid and 4.8g of urea are fully ground and mixed, add 12.96g of dry cornstarch, mix evenly again, add a mixture of 3.5g of deionized water and 1.30g of benzyl alcohol, stir and mix evenly in a mixing cup, put Put it into an oven at 100° C. for 10 h to obtain a crude product of benzyl hydrophobized starch sulfate. Add 50g of deionized water to the crude product to dissolve it, precipitate it with anhydrous methanol, wash it three times with 90% methanol aqueous solution, and dry the filter cake at 50°C for 4 hours to obtain a sulfonic acid group substitution degree of 0.54, benzyl substitution degree 0.04 benzyl hydrophobized starch sulfate.

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Abstract

The invention relates to a preparation method and an application of a hydrophobic starch sulfate ester in a cement water-reducing agent, and belongs to the fields of chemistry and chemical engineering. The preparation method comprises the following steps: adding a sulfamic acid, starch, urea, aliphatic tertiary alcohol or aryl methyl alcohol and water into a reactor under the conditions that the molar ratio of the sulfamic acid to the starch is (0.5-3.0):1, the molar ratio of the urea to the starch is (0.1-3.0):1, the molar ratio of the aliphatic tertiary alcohol or the aryl methyl alcohol to the starch is (0.1-1) and the adding amount of the water accounts for 10% to 30% of the dry weight of the starch; and reacting for 1 to 10 hours at a temperature of 80 DEG C to 150 DEG C, thereby obtaining the hydrophobic starch sulfate ester in which the sulfonyl substitution degree is between 0.04 and 0.89 as well as the alkyl substitution degree is between 0.01 and 0.2. The hydrophobic starch sulfate ester is applied to the cement water-reducing agent, wherein the mass percent of the hydrophobic starch sulfate ester accounts for 0.1% to 1.0% of that of cement. According to the method, a dry method and one-pot reaction are adopted, so that the environmental pollution caused by the application of an organic solvent is avoided. Thus, the production cost is decreased.

Description

technical field [0001] The invention relates to a method for preparing hydrophobized starch sulfate and its application in cement water reducer, belonging to the field of chemistry and chemical engineering. Background technique [0002] Starch is a cheap, easy-to-obtain, non-polluting and renewable natural polymer compound. With the decrease of petroleum resources, the development and utilization of starch and its derivatives have attracted more and more attention from the society, and their application fields have become increasingly extensive. [0003] Starch sulfate was developed as early as the 1950s. Starch sulfate is an anionic starch derivative obtained by introducing sulfonic acid groups on the hydroxyl groups of starch molecules, and it is also an important starch derivative. At present, the preparation method of starch sulfate can be divided into water solvent method, organic solvent method and dry method according to different solvents used; sulfonating agent can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/02C04B24/38C04B103/30
Inventor 张淑芬具本植
Owner DALIAN UNIV OF TECH
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