Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for recycling caustic alkali in sulfonation alkali fusion process

A technology of caustic alkali and sulfonated alkali, applied in chemical instruments and methods, inorganic chemistry, alkali metal compounds, etc., can solve the problems of high material viscosity, difficult extraction, separation or filtration, etc., and achieve low cost and high manufacturing cost The effect of reducing and reducing consumption

Active Publication Date: 2020-06-26
ZHEJIANG LONGSHENG CHEM RES +1
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the azeotropic dehydration of the alkali melt described in the article can separate H acid and sodium hydroxide well after ethanol extraction, our experiments have proved that the material after azeotropic dehydration is very viscous and basically presents a coking state, mainly After the water is removed, the remaining organic matter and salt cannot form a suitable dispersion state, and it is difficult to achieve subsequent extraction, separation or filtration
[0007] In addition to the above patent documents, there are few domestic and foreign literature reports on the separation method of caustic alkali in the alkali fusion production process of aromatic sulfonate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for recycling caustic alkali in sulfonation alkali fusion process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: (methanol+n-heptanol+2-naphthol alkali melt)

[0034] The composition of the alkali fusion product is: 2-naphthol sodium 15.98% (M166), sodium hydroxide 1.08%, sodium sulfate and sodium sulfite 24.12%, water 56.96%, impurity 1.86% (impurity refers to containing sulfonic acid group, amino group, nitrate Naphthalene derivatives).

[0035] Add 100.89g of alkali melt into a 500ml flask, start stirring, then add 16.99g of methanol, heat up to 55-60°C, stir and disperse for 0.5h, then add 100.35g of n-heptanol, stir and extract at 55-60°C for 0.5h , separated after extraction to obtain 99.89g of water phase and 116.71g of organic phase, the content of sodium 2-naphthol in the organic phase was less than 0.1%.

[0036] 5.21 g of water was added to the organic phase, 15.21 g of methanol was distilled off, and 99.18 g of heptanol was obtained by layering, and 5.17 g of an aqueous phase was obtained, wherein the content of sodium hydroxide was 12.61%, and the recov...

Embodiment 2

[0037] Embodiment 2: (ethanol+n-nonanol+J acid-base melt)

[0038] Using 2-naphthylamine-5,7-sodium disulfonate as raw material, 2-naphthylamine-5-hydroxyl-7-sulfonic acid is prepared through alkali fusion and acidification.

[0039] The composition of alkali fusion product is: Sodium J acid 13.51% (M283), sodium hydroxide 15.21%, sodium sulfate and sodium sulfite 13.91%, water 53.59%, impurity 3.78% (impurity refers to containing sulfonic acid group, amino group, nitro class Naphthalene derivatives).

[0040] Add 100.99g of alkali melt into a 500ml flask, start stirring, then add 60.98g of ethanol, raise the temperature to 55-60°C, stir and disperse for 0.5h, then add 300.89g of n-nonanol, stir and extract at 55-60°C for 0.5h , layered after extraction to obtain 84.12g of water phase and 376.81g of organic phase, the content of sodium Jate in the organic phase was less than 0.1%.

[0041] 25.51 g of water was added to the organic phase, 58.72 g of ethanol was distilled off,...

Embodiment 3

[0042] Embodiment 3 (methanol+octanol+resorcinol alkali melt)

[0043] Sodium resorcinol is used as raw material, and resorcinol is prepared through alkali fusion and acidification.

[0044]The composition of alkali fusion product is: resorcinol sodium salt 12.14% (M154), sodium hydroxide 17.42%, sodium sulfate and sodium sulfite 25.41%, water 39.94%, impurity 5.09% (impurity refers to containing sulfonic acid group, hydroxyl class derivative).

[0045] Add 100.53g of alkali melt into a 500ml flask, start stirring, then add 50.98g of methanol, heat up to 55-60°C, stir and disperse for 0.5h, then add 200.79g of octanol, stir and extract at 55-60°C for 0.5h, After extraction, separate layers to obtain 82.06g of water phase and 268.51g of organic phase, the content of resorcinol sodium salt in the organic phase is less than 0.1%.

[0046] 30.59 g of water was added to the organic phase, 48.88 g of methanol was distilled off, and 198.76 g of octanol was obtained by layering, and...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for recycling caustic alkali in a sulfonation alkali fusion process, which comprises the following steps of: (1) pre-dispersing: adding C1-C4 lower alcohol into an aromatic sulfonate alkali fusion product serving as a raw material, stirring and dispersing to obtain dispersion liquid, with the weight of the added lower alcohol being 0.1-1 time of the weight of the alkali fusion product; (2) extracting and layering: adding C6-C12 organic alcohol into the dispersion liquid obtained in the step (1), stirring and extracting, and separating out an organic phase containing caustic alkali at the upper layer and a water phase containing phenate at the lower layer, with the weight of the added C6-C12 organic alcohol being 0.5-5 times of the weight of the alkali fusion reactant; and (3) recycling caustic alkali: adding water into the upper organic phase obtained in the step (2) to control the mass concentration of the recycled alkali to be 20-40%, distilling to remove the lower alcohol to realize natural layering, the upper layer being the C6-C12 organic alcohol, and the lower layer being caustic alkali liquid. The method has the advantages of being high in operability, economical and effective, and recycling of sulfonation alkali fusion process resources is achieved.

Description

[0001] (1) Technical field [0002] The invention relates to a method for recycling caustic alkali in the sulfonated alkali fusion process, in particular to a method for recycling sodium hydroxide or potassium hydroxide in the alkali fusion process in the preparation process of phenolic compounds. [0003] (2) Background technology [0004] Alkali fusion is an important operation unit in chemical reactions. It is usually used to prepare phenolic compounds by eutectically melting aryl sulfonate with sodium hydroxide or potassium hydroxide to convert sulfonic acid groups into hydroxyl groups. For example, some amino polysulfonic acids of the naphthalene series, when caustic alkali is used for alkali fusion, can make a sulfonic acid group in the polysulfonic acid be replaced by a hydroxyl group, while amino and other sulfonic acid groups are not affected, and can prevent amino Hydrolysis and thermal decomposition of naphthyl ketones to obtain higher yields, suitable for alkali fus...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C01D1/34
CPCC01D1/34
Inventor 陶建国方叶明杨日升孟明朱敬鑫苏建军何豪华
Owner ZHEJIANG LONGSHENG CHEM RES