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Method for cooperatively producing 1-naphthol and 2-naphthol from naphthalene sulfonation product by virtue of direct alkali fusion

A product, naphthol technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of repeated investment, serious corrosion of equipment, difficult treatment of filtered wastewater, etc., and achieve energy saving and human resources, closed The effect of a thorough improvement in operation and a thorough improvement in the operating environment

Active Publication Date: 2015-06-10
肖刚学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent consumes the acid mother liquor of 1-naphthalenesulfonic acid through high-temperature sulfonation synthesis of 2-naphthalenesulfonic acid, but a large amount of mother liquor wastewater after neutralization and crystallization of 2-naphthalenesulfonic acid still cannot be solved; the acid mother liquor of 1-naphthalenesulfonic acid is in Separation at 5°C requires high energy consumption, and the concentration of the acid mother liquor is low, which seriously corrodes the equipment; separately preparing 1-naphthalenesulfonic acid and 2-naphthalenesulfonic acid and entering into the processes of neutralization, filtration and alkali fusion respectively, resulting in cumbersome operations , repeated investment
[0007] In addition to their own inherent defects, the above-mentioned various process methods all present the common shortcomings of a large amount of filtered wastewater that is difficult to treat, complex procedures, long process flow, and high energy consumption.

Method used

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  • Method for cooperatively producing 1-naphthol and 2-naphthol from naphthalene sulfonation product by virtue of direct alkali fusion
  • Method for cooperatively producing 1-naphthol and 2-naphthol from naphthalene sulfonation product by virtue of direct alkali fusion

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Sulfonation: Add 260.4 grams of naphthalene into a 500ml three-neck flask, heat up to about 80°C and start stirring after the naphthalene melts. At 80-90°C, add concentrated sulfuric acid dropwise according to the acid-naphthalene molar ratio of 1.1:1, and keep the reaction at 90-100°C for 3 hours. Distill under reduced pressure for 60 minutes at 85-95°C with a vacuum degree of 0.025-0.045Mpa. Then add naphthalene according to the total molar ratio of naphthalene to concentrated sulfuric acid 1.8:1, and keep reacting at 90-100°C for 3 hours. Distill under reduced pressure for 90 minutes at 85-95°C with a vacuum of 0.025-0.045MPa. The obtained liquid mixture of sulfonated products 1-naphthalenesulfonic acid and 2-naphthalenesulfonic acid is controlled at 90-100°C for alkali fusion.

[0028] (2) Alkali fusion: Add solid sodium hydroxide into the alkali fusion stainless steel pot, heat up to above 210°C and start stirring after complete melting. When the temperature...

Embodiment 2

[0032] (1) Sulfonation: Add 260.4 grams of naphthalene into a 500ml three-neck flask, heat up to about 80°C and start stirring after the naphthalene melts. Add concentrated sulfuric acid dropwise at 150-160°C according to the acid-naphthalene molar ratio of 1.6:1, and keep reacting for 2 hours at 155-165°C. Distill under reduced pressure at 150-160° C. for 30 minutes with a vacuum degree of 0.01-0.025 MPa. Then add naphthalene according to the total molar ratio of naphthalene to concentrated sulfuric acid 1.3:1, and keep reacting for 1 hour at 155-165°C. Distill under reduced pressure for 60 minutes at 150-160°C with a vacuum of 0.01-0.025MPa. The obtained liquid mixture of sulfonated products 1-naphthalenesulfonic acid and 2-naphthalenesulfonic acid is controlled at 150-160°C for alkali fusion.

[0033](2) Alkali fusion: Add solid sodium hydroxide into the alkali fusion stainless steel pot, heat up to above 210°C and start stirring after complete melting. When the temperat...

Embodiment 3

[0037] According to the technical process described in embodiment 1

[0038] (1) Sulfonation: Add 260.4 grams of naphthalene into a 500ml three-neck flask, heat up to about 80°C and start stirring after the naphthalene melts. Add concentrated sulfuric acid dropwise at 85-90°C according to the acid-naphthalene molar ratio of 1.2:1, and keep the reaction at 115-125°C for 2.5 hours. Distill under reduced pressure for 100 minutes at 120-123°C with a vacuum of 0.045-0.05MPa. Then add naphthalene according to the total molar ratio of naphthalene to concentrated sulfuric acid 1.5:1, and keep the reaction at 115-125°C for 2 hours. Distill under reduced pressure for 90 minutes at 130-133°C with a vacuum of 0.085-0.09MPa. Keep the obtained liquid mixture of sulfonated products 1-naphthalenesulfonic acid and 2-naphthalenesulfonic acid at 110-120°C for alkali fusion.

[0039] (2) Alkali fusion: Add solid sodium hydroxide into the alkali fusion stainless steel pot, heat up to above 210°...

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Abstract

The invention discloses a method for cooperatively producing 1-naphthol and 2-naphthol from a naphthalene sulfonation product by virtue of direct alkali fusion. The method comprises the following steps: performing multiple sulfonation reactions on naphthalene and concentrated sulfuric acid, directly performing an alkali fusion reaction on the obtained liquid sulfonation product and sodium hydroxide in a molten state, and then diluting, acidifying, boiling for layering, dehydrating and drying, rectifying and separating, thereby obtaining high-purity 1-naphthol and 2-naphthol simultaneously. The steps of hydrolyzing, naphthalene blowing, neutralization, cooling and crystallization and filtration of sulfonation products, and feeding for performing alkali fusion on a water-containing filter cake at a normal temperature in the existing process are avoided; no filtration wastewater difficult to treat is not generated anymore, the energy source and the resources are saved, the yield is increased and the operating environment is improved; as a result, the problems of three-waste treatment during naphthol production are thoroughly solved from the production process.

Description

technical field [0001] The present invention relates to a kind of preparation method of coproduction 1-naphthol and 2-naphthol, especially relate to a kind of naphthalene sulfonation product directly and molten sodium hydroxide to carry out alkali fusion reaction coproduction 1-naphthol and 2-naphthol The method of phenol is also a clean production method of naphthol without waste water. technical background [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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/04C07C39/14
Inventor 肖刚学
Owner 肖刚学
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