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Beta-naphthol produced waste liquid modified amido sulfoacid series high-efficiency water reducer and preparation method thereof

A sulfamic acid-based, high-efficiency water-reducing agent technology, applied in the field of building materials, to achieve good workability, easy control of reaction conditions, and obvious enhancement effects

Active Publication Date: 2010-09-08
NANJING RUIDI HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far there is no report about directly using β-naphthol to produce waste liquid modified sulfamic acid series high-efficiency water reducer,

Method used

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  • Beta-naphthol produced waste liquid modified amido sulfoacid series high-efficiency water reducer and preparation method thereof
  • Beta-naphthol produced waste liquid modified amido sulfoacid series high-efficiency water reducer and preparation method thereof

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preparation example Construction

[0020] The preparation process steps of the preparation method of the high-efficiency water reducer are as follows: each process step is carried out under normal pressure.

[0021] (1) Sulfonation reaction: first add β-naphthol production waste liquid into the reaction kettle, heat it to 105-110°C, add concentrated sulfuric acid dropwise, drop it in 15-30 minutes, and keep it warm for 1.5-2.5 hours to obtain naphthol Sulfonate.

[0022] (2) Polycondensation reaction: Heat water to 65-75°C, add sodium p-aminobenzenesulfonate, phenolic compounds and about three-quarters of the total amount of pH regulator into the reaction kettle, and heat up to 80-90°C; add formaldehyde dropwise, finish dropping within 10-30 minutes, and keep the temperature between 85-95°C, keep warm for 2-5 hours; add the remaining pH regulator and naphthol obtained in step (1) The sulfonate is reacted at 85-95° C. for 1.5-2.5 hours, and then cooled and discharged to obtain a liquid product. The above liqui...

Embodiment 1

[0034] The preparation process of the present invention comprises two steps, and each process step is all carried out under normal pressure:

[0035] (1) Sulfonation reaction: Put 480 kg of β-naphthol production waste liquid into the reaction kettle, heat it to 110°C, add 120 kg of concentrated sulfuric acid dropwise, drop it in 15 minutes, and keep it warm for 2 hours to obtain naphthol sulfonate .

[0036] (2) Polycondensation reaction: Heat water to 70°C, add 419 kg of sodium p-aminobenzenesulfonate, 475 kg of phenol and 75 kg of sodium hydroxide into the reaction kettle, heat up to 85°C while stirring; add 720 kg of formaldehyde dropwise , dripped within 20 minutes, and kept the temperature at 95°C for 2.5 hours; added the remaining 30 kg of sodium hydroxide and the naphthol sulfonate obtained in step (1), reacted at 95°C for 1.5 hours, then cooled and discharged , that is, a liquid product is prepared. The above-mentioned liquid product is then spray-dried to obtain a p...

Embodiment 2

[0038] The preparation process of the present invention comprises two steps, and each process step is all carried out under normal pressure:

[0039] (1) Sulfonation reaction: put 390 kg of β-naphthol production waste liquid into the reaction kettle, heat it to 105°C, add 114 kg of concentrated sulfuric acid dropwise, drop it in 15 minutes, and keep it warm for 2 hours to obtain naphthol sulfonate .

[0040] (2) Polycondensation reaction: Heat water to 70°C, add 405 kg of sodium p-aminobenzenesulfonate, 526 kg of bisphenol A, 12 kg of calcium hydroxide and 60 kg of potassium hydroxide into the reaction kettle, and heat up to 85°C; add 685 kg of formaldehyde dropwise, drop it within 20 minutes, and keep the temperature at 90°C for 3 hours; add the remaining 33 kg of potassium hydroxide and the naphthol sulfonate obtained in step (1), at 95°C After reacting for 2 hours, the temperature was lowered and the material was discharged to obtain a liquid product.

[0041] The followi...

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Abstract

The invention relates to a beta-naphthol produced waste liquid modified amido sulfoacid series high-efficiency water reducer and a preparation method thereof, wherein the preparation method comprises the following preparation steps of: a. sulfonation reaction: firstly adding a beta-naphthol produced waste liquid into a reaction kettle, heating to the temperature of 105-110 DEG C, dropwise adding concentrated sulfuric acid for 15-30 minutes and preserving heat for 1.5-2.5 hours to obtain naphthol sulfonate; b. polycondensation reaction: heating water to the temperature of 65-75 DEG C, adding sodium p-aminobenzenesulfonate, a phenol compound and a pH value regulator which accounts for about three fourths of the gross amount into the reaction kettle and increasing the temperature to 80-90 DEG C while stirring; dropwise adding formaldehyde for 10-30 minutes, keeping the temperature at 85-95 DEG C and preserving heat for 2-5 hours; and adding the residual pH value regulator and the naphthol sulfonate obtained in step a, reacting at the temperature of 85-95 DEG C for 1.5-2.5 hours, then reducing the temperature and discharging to prepare a liquid product. When the doped amount of the prepared modified amido sulphate high-efficiency water reducer is 0.3-0.8 percent (calculated by solids) of the mass of a cementing material, the corresponding water reducing rate is 16-24 percent.

Description

technical field [0001] The invention relates to a high-efficiency concrete water-reducer and its preparation method, more specifically, a sulfamate high-efficiency water-reducer prepared by modifying the waste liquid produced by β-naphthol as a raw material, which belongs to building materials technology field. Background technique [0002] Concrete water reducer is an important component of high performance concrete. At present, in the domestic market, the high-efficiency water-reducing agents are mainly naphthalene-based and polycarboxylic acid-based water-reducing agents. The latter is mainly used in high-performance concrete such as passenger dedicated lines because of its high price. Sulfonic acid-based high-efficiency water reducer, etc. The disadvantages of naphthalene-based water-reducers are large slump loss and prone to crystal precipitation in low-temperature environments; the high price of new polycarboxylate-based water-reducers affects their wide application;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/24C08G8/18C04B24/22C04B103/30
Inventor 陈国新祝烨然王冬唐修生蔡明黄国泓付丹华
Owner NANJING RUIDI HIGH TECH
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