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A method for producing naphthalene-based water-reducers by centralized sulfonation and meal-divided condensation by solvent method

A naphthalene-based water-reducing agent and centralized sulfonation technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of large area, low production efficiency, heat loss, etc., to reduce solvent usage, reduce steam usage, Avoid the effect of alternating hot and cold

Active Publication Date: 2018-06-08
山东汶河新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its production process is mainly to put industrial naphthalene into the reaction kettle, heat up to a certain temperature, add concentrated sulfuric acid dropwise while stirring for sulfonation, keep warm, hydrolyze, add formaldehyde to condense, neutralize, and dry. At present, the general production method The sulfonation is carried out in a 5 cubic reaction kettle. After the sulfonation is completed, formaldehyde is condensed dropwise in the same reaction kettle. This operation has the following four problems: (1) In large-scale production, due to the alternating refrigerant and heat medium (2) The heat loss in a single batch operation is serious, and the heat released by the reaction is not fully utilized; (3) The reaction area is large, and the exhaust gas volatilizes a large amount; (4) The production efficiency is low, and continuous production cannot be realized; (5) When industrial naphthalene is sulfonated with sulfuric acid, especially when high-concentration sulfuric acid is used, such as 100%, 105%, 120% and other high-concentration concentrated sulfuric acid, the concentrated sulfuric acid cannot be dispersed in time, and it is easy to produce di Sulfonic acid or polysulfonic acid reduces the selectivity of β-naphthalenesulfonic acid, affects the next step of formaldehyde condensation, and affects the quality of the water reducer

Method used

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  • A method for producing naphthalene-based water-reducers by centralized sulfonation and meal-divided condensation by solvent method
  • A method for producing naphthalene-based water-reducers by centralized sulfonation and meal-divided condensation by solvent method
  • A method for producing naphthalene-based water-reducers by centralized sulfonation and meal-divided condensation by solvent method

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Embodiment 1

[0044] The embodiment of the present disclosure provides a method for producing naphthalene-based water-reducers by concentrated sulfonation and meal-divided condensation using a solvent method, such as figure 1 shown, including the following steps:

[0045] S101: Feeding: Add 5000kg of liquid naphthalene to a 12.5m³ reactor, and heat up with steam;

[0046] S102: Sulfonation: When the temperature of liquid naphthalene rises to 140°C, start to slowly and uniformly add 4250kg of 98% concentrated sulfuric acid, and finish adding in 60 minutes. After adding the acid, continue to heat up with steam, heat up to 160°C and keep it warm for 4 hours to carry out sulfonation reaction ;

[0047] S103: Dehydration: Continuously pump ethyl acetate solvent into the reaction solution in step S102, the solvent will bring out the water produced by the sulfonation reaction when the solvent volatilizes at high temperature, and after condensation, the water and the ethyl acetate solvent will be ...

Embodiment 2

[0052] The embodiment of the present disclosure provides a method for producing naphthalene-based water-reducers by concentrated sulfonation and meal-divided condensation using a solvent method, such as figure 1 shown, including the following steps:

[0053] S101: Feeding: add 5200kg of liquid naphthalene to the 20m³ reactor, and heat up with steam;

[0054] S102: Sulfonation: When the temperature of liquid naphthalene rises to 145°C, add 3,380kg of 98% concentrated sulfuric acid slowly and uniformly, and finish adding in 70 minutes. After adding acid, continue to heat up with steam, heat up to 165°C and keep it warm for 2.5h, then carry out sulfonation reaction;

[0055] S103: Dehydration: Continuously pump xylene solvent into the reaction liquid in step S102, and the water generated by the sulfonation reaction will be taken out when the solvent volatilizes at high temperature. After condensation, the water and xylene solvent will be separated, and the separated solvent will...

Embodiment 3

[0060] The embodiment of the present disclosure provides a method for producing naphthalene-based water-reducers by concentrated sulfonation and meal-divided condensation using a solvent method, such as figure 1 shown, including the following steps:

[0061] S101: Feeding: add 5200kg of liquid naphthalene to the 20m³ reactor, and heat up with steam;

[0062] S102: Sulfonation: When the temperature of liquid naphthalene rises to 145°C, add 3,380kg of 98% concentrated sulfuric acid slowly and uniformly, and finish adding in 70 minutes. After adding acid, continue to heat up with steam, heat up to 165°C and keep it warm for 2.5h, then carry out sulfonation reaction;

[0063] S103: Dehydration: Continuously pump xylene solvent into the reaction liquid in step S102, and the water generated by the sulfonation reaction will be taken out when the solvent volatilizes at high temperature. After condensation, the water and xylene solvent will be separated, and the separated solvent will...

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Abstract

The invention provides a method for solvent method centralized sulfonation separate type condensation production of a naphthalene water reducer. The method includes the steps of putting, sulfonation, dehydration, hydrolysis, condensation, neutralization and the like. By adopting a low acid blending amount for sulfonation, no disulfonic acid or polysulfonic acid is generated, the selectivity of beta-naphthyl sulfonic acid is improved, the quality of the water reducer is improved, and the emission of waste residues is reduced; solvent is used in the sulfonation process, the water outlet amount serves as the reaction endpoint target value, the solvent amount for each time of dehydration is gradually reduced, the solvent use amount is reduced to the maximum, and thus the heat loss is reduced; a large-volume reaction kettle is adopted for centralized sulfonation, reaction released heat is fully utilized, the temperature of the reaction kettle is kept, and the steam use amount is reduced; the emission of waste gas is reduced; condensation is carried out without pressure, and thus safety is high.

Description

technical field [0001] The invention relates to the technical field of concrete admixture production, in particular to a method for producing naphthalene-based water-reducers through centralized sulfonation and meal-dividing condensation by solvent method. Background technique [0002] Water reducer is a concrete admixture that can reduce the amount of mixing water while maintaining the slump of concrete. Most of them are anionic surfactants, such as lignosulfonate, naphthalenesulfonate formaldehyde polymer, etc. After being added to the concrete mixture, it can disperse the cement particles, improve its workability, reduce the unit water consumption, improve the fluidity of the concrete mixture; or reduce the unit cement consumption and save cement. [0003] Naphthalene-based water reducer is a widely used high-efficiency water reducer. It is a superplasticizer with good water-reducing and early-strength effects. It is mostly used in the concrete industry, and is also used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G16/02C04B24/22C07C303/06C07C309/35C04B103/30
CPCC04B24/226C04B2103/302C07C303/06C08G16/0237C07C309/35
Inventor 亓建设李坤笃李宏石张修利孙燕杰张留军时军祥张务云杨秀云张仲禄吴修平
Owner 山东汶河新材料有限公司