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A kind of sulfonation method of naphthalene

A sulfonation, one-time technology, applied in the direction of sulfonic acid preparation, organic chemistry, etc., can solve the problems of lower production efficiency, can not truly reflect the content or purity of sulfonated material, large error, etc., achieve good application effect, shorten the production time of sulfonate The effect of saving time and improving production efficiency

Inactive Publication Date: 2014-10-15
ZHEJIANG LONGSHENG GROUP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional sulfonation process of naphthalene-based water reducer is to use industrial naphthalene and sulfuric acid to mix according to a certain ratio, and keep warm at 160-170°C for 2-3 hours for sulfonation reaction, because the fluidity of cement slurry is the best during this period of time. Yes, the product has good performance. If the sulfonation time is too long, it will not only reduce the production efficiency, but also easily produce isomers such as naphthalene disulfonic acid
A common test method is to test the acidity of the sulfonated material. This test method has too much error, and it cannot truly reflect the content or purity of each substance in the sulfonated material, and cannot indicate the progress of the reaction.

Method used

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  • A kind of sulfonation method of naphthalene
  • A kind of sulfonation method of naphthalene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Preparation of Cr-SO by Sol-Gel Method 4 / ZrO 2 The process is as follows:

[0016] 18mL Zr(OCH 2 CH 2 CH 3 ) 4 Dissolve in 60mL of 15% (w / w) aluminum isopropoxide solution, add 30mL of isopropanol and 4mL of water, add nitric acid (65%, w / w, 0.6mL) as catalyst, and keep stirring (25°C) for 30min, The obtained zirconium hydroxide sol was aged at 40°C for 24 hours to complete the polycondensation reaction, and the resulting gel was slowly dried at 150°C to obtain a highly hydrated amorphous gel. Grinding to 200 mesh, soaking in (sulfuric acid / potassium dichromate=2mol / 1mol) / L potassium dichromate sulfuric acid solution (70°C) for 24h, drying at 500-550°C for 3h, the specific surface area can be obtained Up to 228m 2 / g Cr-SO 4 / ZrO 2 Solid super acid.

Embodiment 2

[0018] Weigh 2400kg of industrial naphthalene with a content of 96%, 2700kg of 98% concentrated sulfuric acid, and make Cr-SO 4 / ZrO 2 0.3kg of solid super acid, 50kg of anhydrous sodium sulfate; put industrial naphthalene into the sulfonation reactor, raise the temperature to 140°C, add concentrated sulfuric acid, raise the temperature to 169°C, react for 0.5 hours, cool down to 120°C, and take samples for HPLC detection Naphthalene content, purity of β-naphthalenesulfonic acid and purity of double sulfonates (results see figure 1 ), and then transferred to the condensation kettle.

[0019] At 120°C, pass 155°C high-temperature steam into the condensation kettle for hydrolysis and recovery of naphthalene homologues; stop feeding steam after 45 minutes, add 300kg of water, adjust the temperature to 100°C, and then add 1420kg of formaldehyde After condensing for 5 hours, transfer the material to a neutralization tank, add 30-32% NaOH aqueous solution, adjust the pH value to 7...

Embodiment 3

[0021] Weigh 2400kg of industrial naphthalene with a content of 97.5%, 2750kg of 98% concentrated sulfuric acid, and make Cr-SO 4 / ZrO 2 0.35kg of solid super acid, 60kg of anhydrous sodium sulfate; put industrial naphthalene into the sulfonation reactor, raise the temperature to 140°C, add concentrated sulfuric acid, raise the temperature to 166°C, react for 1 hour, cool down to 120°C, and take samples for HPLC detection The content of naphthalene, the purity of β-naphthalenesulfonic acid and the purity of double sulfonates are then transferred to the condensation reactor.

[0022] At 120°C, pass 155°C high-temperature steam into the condensation kettle for hydrolysis and recovery of naphthalene homologues; stop feeding steam after 45 minutes, add 300kg of water, adjust the temperature to 100°C, and then add in proportion After condensing 1450kg of formaldehyde for 5 hours, transfer the material to the neutralization tank, add 30-32% NaOH aqueous solution, adjust the pH valu...

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Abstract

The invention relates to a method for sulfonating naphthalene, in particular to the method for sulfonating naphthalene in a naphthalene formaldehyde water reducer preparation process. The method comprises the following steps of: (1) dropwise adding measured concentrated sulfuric acid of which the concentration is 98 percent into melted naphthalene at the temperature of 140 to 165 DEG C within 45 minutes, wherein the mass ratio between the industrial naphthalene and the concentrated sulfuric acid is 1:(1-1.3); and (2) after the concentrated sulfuric acid is dropwise added, adding measured mixture of solid super acid and anhydrous sodium sulfate into the naphthalene, wherein the solid super acid is Cr-SO4 / ZrO2, the mass using amount of the solid super acid is 0.01 to 0.2 percent that of the sulfuric acid, and the mass using amount of the anhydrous sodium sulfate is 1 to 3 percent that the sulfuric acid, preserving the heat and sulfonating for 0.5 to 1.5 hours at 160 to 170 DEG C to obtain the naphthalene sulfonic acid. The method has the main beneficial effects that: in a production process, even the sulfonating time is shortened, the production efficiency can still be improved, and the obtained product has a very good application effect at the same time.

Description

(1) Technical field [0001] The invention relates to a naphthalene sulfonation method, in particular to a naphthalene sulfonation method in the preparation process of a naphthalene-based water reducer. (2) Background technology [0002] The sulfonation process is one of the important steps in the production process of naphthalene-based superplasticizers, and the sulfonation time in the sulfonation process has a certain impact on the by-products generated by the product. The traditional sulfonation process of naphthalene-based water reducer is to use industrial naphthalene and sulfuric acid to mix according to a certain ratio, and keep warm at 160-170°C for 2-3 hours for sulfonation reaction, because the fluidity of cement slurry is the best during this period of time. Yes, the product has good performance. If the sulfonation time is too long, it will not only reduce the production efficiency, but also easily produce isomers such as naphthalene disulfonic acid. A common test ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/35C07C303/06
Inventor 金瑞浩韩玉龙
Owner ZHEJIANG LONGSHENG GROUP
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