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Naphthalene sulfonating method for coproducing 1-naphthol and 2-naphthol

A naphthol and sulfonation technology is applied in the field of naphthalene sulfonation for co-production of 1-naphthol and 2-naphthol, and can solve the problems of easily destroyed 1-naphthalenesulfonic acid, high concentration of naphthalenesulfonic acid solution and high equipment requirements , to achieve the effect of improving yield and purity, reducing production costs, and simplifying production processes

Inactive Publication Date: 2018-09-14
山西豪仑科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are also many methods to utilize 1-naphthalenesulfonic acid to generate 1-naphthol, but in the process of adding sodium sulfite solution to the naphthalenesulfonic acid melt during neutralization in the traditional process, it is easy to destroy 1-naphthalenesulfonic acid. The concentration of sulfonic acid solution is high, the acidity is strong, and the requirements for equipment are relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] a) Sulfonation: React naphthalene with concentrated sulfuric acid at 120°C for 2 hours to obtain molten naphthalenesulfonic acid;

[0020] b) Neutralization: First add 12% sodium sulfite solution into the neutralization kettle, then add the naphthalenesulfonic acid molten material into the neutralization kettle, adjust the pH to 1, heat the solution to 105°C, and keep it warm for 15 minutes to make the SO 2 The volatilization was complete, and after the reaction was finished, the pH of the neutralization tank was adjusted to be 7 using sodium hydroxide. The method of adding the naphthalenesulfonic acid molten material is to divide the naphthalenesulfonic acid molten material into three parts and add them step by step. The time ratio of adding the three parts of naphthalenesulfonic acid molten material from front to back is 2:1:3.

[0021] After neutralization, blowing naphthalene, crystallization at lower temperature, filtration, alkali fusion, dilution, acidification, ...

Embodiment 2

[0023] a) Sulfonation: React naphthalene with concentrated sulfuric acid at 150°C for 5 hours to obtain molten naphthalenesulfonic acid;

[0024] b) Neutralization: first add 12% sodium sulfite solution into the neutralization kettle, then add the naphthalenesulfonic acid molten material into the neutralization kettle, adjust the pH to 2, heat the solution to 105°C, and keep it warm for 15 minutes to make the SO 2 Volatilize completely, after the reaction finishes, use sodium hydroxide to adjust the pH of the neutralization tank to be 8; the method of adding the naphthalenesulfonic acid molten material is to divide the naphthalenesulfonic acid molten material into three parts and add step by step, three parts of naphthalenesulfonic acid melt The time ratio of feeding materials from front to back is 2:1:2.

[0025] After neutralization, blow naphthalene, crystallize by cooling, filter, alkali fusion, dilute, acidify, boil and separate, dehydrate and dry, and rectify and separat...

Embodiment 3

[0027] a) Sulfonation: React naphthalene with concentrated sulfuric acid at 130°C for 4 hours to obtain molten naphthalenesulfonic acid;

[0028] b) Neutralization: first add 12% sodium sulfite solution into the neutralization kettle, then add the naphthalenesulfonic acid molten material into the neutralization kettle, adjust the pH to 2, heat the solution to 105°C, and keep it warm for 15 minutes to make the SO 2 The volatilization is complete. After the reaction is over, use sodium hydroxide to adjust the pH of the neutralization tank to be 7. The method of adding the naphthalenesulfonic acid molten material is to divide the naphthalenesulfonic acid molten material into three parts and add it step by step. Three parts of naphthalenesulfonic acid melt The time ratio of feeding materials from front to back is 2:1:2.5.

[0029] After neutralization, blow naphthalene, crystallize by cooling, filter, alkali fusion, dilute, acidify, boil and separate, dehydrate and dry, and rectif...

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PUM

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Abstract

The invention discloses a naphthalene sulfonating method for coproducing 1-naphthol and 2-naphthol. The naphthalene sulfonating method comprises the following steps: directly neutralizing after carrying out sulfonating reaction: adding a sodium sulfite solution of which the concentration is 12 percent into a neutralizing kettle, then adding a naphthalene sulfonic acid molten material, reacting byregulating PH (Potential of Hydrogen) to be 1 to 2, heating the solution to be 105 DEG C, keeping warm for 15 minutes, and regulating the PH of the neutralizing kettle to be 7 to 8 after completing reaction; after neutralizing, sequentially carrying out naphthalene blowing, cooling crystallization, filtering, alkaline fusion, diluting, acidifying, boiling and stratifying, dewatering and drying and distillation separation, thus generating 1-naphthol and 2-naphthol. According to the naphthalene sulfonating method disclosed by the invention, a 1-naphthalene sulfonic acid isomer in a sulfonatingproduct does not need to be removed, 1-naphthol and 2-naphthol are simultaneously obtained through co-production, and the yield and the purity of 1-naphthol and 2-naphthol are effectively increased through specific production steps; a hydrolysis step is omitted, generation of wastewater during production is reduced, a production technology is simplified, and the production cost is reduced.

Description

technical field [0001] The present invention relates to a naphthalene sulfonation method for co-production of 1-naphthol and 2-naphthol, in particular to a naphthalene sulfonation method for co-production of 1-naphthol and 2-naphthol through direct neutralization of naphthalene sulfonation products method. Background technique [0002] 1-Naphthol, commonly known as methylnaphthol, also known as α-naphthol, is currently mainly used as an intermediate for the pesticide carbaryl, and can also be used as an intermediate for some drugs and fine chemical products. Its production mainly adopts naphthalene nitration, reduction, and hydrolysis methods. Since about 4% of 2-nitronaphthalene is produced during nitration, the general product content is about 96%, so it is necessary to obtain a content that meets the national standard GB / T3410-2002 to reach 99.5% % of high-quality product 1-naphthol needs to adopt nitronaphthalene crystallization separation and purification or product cr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/225C07C37/04C07C303/06C07C303/32C07C309/35
CPCC07C37/04C07C303/06C07C303/32C07C309/35C07C39/225
Inventor 韩喜民马建安李斌革
Owner 山西豪仑科化工有限公司
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