Method for synthesizing dimethyl isophthalate-5-sodium sulfonate

A technology of dimethyl isophthalate and isophthalic acid, which is applied in the field of synthesis of dimethyl isophthalate-5-sodium sulfonate, can solve the problem of demanding equipment anhydrous and affecting product yield and quality , increase in side reactions and other issues, to achieve the effect of reducing the amount of soda ash used, improving production safety, and avoiding the increase in side reactions

Active Publication Date: 2012-08-15
WEIFANG WORLD CHEM
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Problems solved by technology

[0015] But there are still following disadvantages: when sulfur trioxide is sulfonated, it is very easy to form sulfone, resulting in low product purity
Advantages: With SO in oleum 3 With the increase of the content, although the fluidity of the sulfonated product is poor, the reactivity is improved, the sulfonation reaction speed is fast, the reaction temperature is reduced, the reaction time is shortened, and the content of the disulfonic acid on the isophthalic acid is low; Whether the kettle-type intermittent sulfonation process or the tank-type continuous sulfonation process is used, there are problems such as poor mass transfer, slow heat transfer, local overheating, many side reactions, and long reaction time, which also lead to low product purity.
[0018] The advantage of this method is: the production process is easy to control; the disadvantages are: the process flow is long, the two-step esterification reaction increases the side reaction, the product yield is low, the impurity content in the finished product is high, and the product economic benefit is poor
The disadvantages are: two alkali additions are required in production, the process route is long, the product yield is low, the cost is high, and chlorosulfonic acid is hydrolyzed immediately when it meets water, the requirements for anhydrous equipment are harsh, the equipment investment is large, and the price is expensive. HCl has strong corrosive
[0040] In the prior art, a single catalyst is used, and the temperature of the sulfonation reaction is high, and there are various degrees of intense reaction in the early stage, many by-products, a decrease in the reaction activity in the middle and late stages, and a slow increase in the conversion rate of isophthalic acid, which directly affect the product yield. rate and quality

Method used

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  • Method for synthesizing dimethyl isophthalate-5-sodium sulfonate

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Experimental program
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Embodiment 1

[0062] Preparation concentration is the oleum of 64wt%, according to isophthalic acid: oleum: cadmium sulfate: SiO 2 : mercuric sulfate: anhydrous sodium sulfate=1: 0.879: 0.0003: 0.0005: 0.0005: 0.001 The mass ratio of the feed ingredients: first add oleum to the sulfonation kettle at one time, start stirring, add 20% of the total amount of isophthalic acid %, heat the material in the sulfonation tank, raise the temperature of the material to 125°C within 20 minutes, then add all the remaining isophthalic acid to the sulfonation tank, add anhydrous sodium sulfate, and then raise the temperature of the material to 150°C cadmium sulfate was added, and the reaction was kept for 60 minutes; then the temperature of the material was raised to 160°C within 30 minutes, and the reaction was first kept for 20 minutes, and then SiO was added. 2 , and then heat preservation reaction for 60 minutes; finally, within 20 minutes, the temperature of the material was raised to 170°C, and the h...

Embodiment 2

[0067] Preparation concentration is the oleum of 65wt%, according to isophthalic acid: oleum: cadmium sulfate: SiO 2 : mercuric sulfate: anhydrous sodium sulfate=1: 0.885: 0.0006: 0.0009: 0.0009: 0.004 mass ratio ingredients: first add oleum to the sulfonation kettle at one time, start stirring, add 24% of the total amount of isophthalic acid %, heat the material in the sulfonation tank, raise the temperature of the material to 128°C within 24 minutes, then add all the remaining isophthalic acid to the sulfonation tank, add a small amount of anhydrous sodium sulfate, and then raise the temperature of the material to At 153°C, add cadmium sulfate and keep it warm for 70 minutes; then within 35 minutes, the temperature of the material rises to 163°C, first keep it warm for 24 minutes, then add SiO 2 , and then heat preservation reaction for 68 minutes; finally, within 30 minutes, the temperature of the material was raised to 173° C., and the heat preservation reaction was carried ...

Embodiment 3

[0072] Preparation concentration is the oleum of 66wt%, according to isophthalic acid: oleum: cadmium sulfate: SiO 2 : mercury sulfate: anhydrous sodium sulfate = 1: 0.889: 0.0008: 0.0010: 0.0012: 0.008 mass ratio of feed ingredients: first add oleum to the sulfonation kettle at one time, start stirring, add 26% of the total amount of isophthalic acid , heat the material in the sulfonation tank, raise the temperature of the material to 130°C within 28 minutes, then add all the remaining isophthalic acid into the sulfonation tank, and then increase the temperature of the material to 156°C, add cadmium sulfate, and keep warm React for 70 minutes; then within 40 minutes, the temperature of the material rises to 166°C, and the temperature is kept for 28 minutes before adding SiO 2 , and then heat preservation reaction for 75 minutes; finally, within 40 minutes, the temperature of the material was raised to 176°C, and the heat preservation reaction was carried out for 36 minutes, t...

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Abstract

The invention discloses a method for synthesizing dimethyl isophthalate-5-sodium sulfonate. Dimethyl isophthalate-5-sodium sulfonate is prepared by steps of sulfonation reaction, esterification, neutralization reaction and aftertreatment with isophthalic acid and fuming sulfuric acid serving as raw materials, wherein the sulfonation reaction is completed in three reaction temperature zones, different catalysts are used in different reaction temperature zones, cadmium sulfate is used as the catalyst at the temperature ranging from 150 DEG C to 159 DEG C, SiO2 is used as the catalyst at the temperature ranging from 160 DEG C to 169 DEG C, and mercuric sulfate is used as the catalyst temperature ranging from 170 DEG C to 181 DEG C. By the method, sulfonation reaction effect is improved, conversion rate of isophthalic acid is increased, sulfonation reaction temperature is lowered while sulfonation reaction time is shortened, reaction by-products including disulfonate, polymer and sulfone compounds are greatly reduced, product purity is improved while product yield is increased, and further, usage of fuming sulfuric acid and usage of sodium carbonate in a subsequent neutralization procedure are reduced, so that production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing dimethyl isophthalate-5-sodium sulfonate. Background technique [0002] Dimethyl isophthalate-5-sodium sulfonate (commonly known as trimonomer, English abbreviation SIPM), as an important differential modifier for the production of modified polyester products (CDP / ECDP, etc.), adding slices (PET) blended yarn solves the problem of poor hygroscopicity, difficult dyeing, and easy static electricity of conventional polyester determined by the molecular structure of polyester, and when the fiber strength is too high, the fabric is often prone to pilling, and its style and clothing comfort are different from natural fibers. There are many defects such as a large gap. [0003] Introducing SIPM into polyester chips can produce cation-modified polyester filaments. Although its appearance is not much different from ordinary polyester filaments, the col...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/58C07C303/32
Inventor 郭学阳熊激光郭祥荣邢玉贞崔国强张云玲房菲菲朱浩慧李厚强董泮松赵建文王亮单宝来王建玲于庆展
Owner WEIFANG WORLD CHEM
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