A method for producing diethylene glycol isophthalate-5-sodium sulfonate from concentrate of three monomer process wastewater

A concentrated material and three-monomer technology, applied in the preparation of sulfonate, organic chemistry, etc., can solve the problems of easy precipitation of solids, high content of sulfate ions, poor stability of SIPE solution, etc., and achieve less impurity content and good stability , the effect of high purity

Active Publication Date: 2021-05-28
SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI +1
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  • Abstract
  • Description
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Problems solved by technology

[0013] (1) The three-monomer wastewater concentrated solid material has complex components, which contain a certain amount of sodium sulfate, which makes the prepared SIPE have a high content of sulfate ions, which affects the appearance and quality of SIPE and its synthesized polyester; It will further affect the broken filament rate of polyester finished spinning, the clogging of precision filters during spinning and the length of cleaning and replacement cycles.
[0014] (2) The composition of the three-monomer wastewater concentrate is complex. When reacting with ethylene glycol to prepare SIPE, esterification and transesterification reactions occur simultaneously. The reaction temperature and reaction time have a great influence on the quality and purity of the product.
[0016] (3) The SIPE solution prepared by the prior art has poor stability, is easy to precipitate solids, and the quality index is easy to change

Method used

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  • A method for producing diethylene glycol isophthalate-5-sodium sulfonate from concentrate of three monomer process wastewater
  • A method for producing diethylene glycol isophthalate-5-sodium sulfonate from concentrate of three monomer process wastewater
  • A method for producing diethylene glycol isophthalate-5-sodium sulfonate from concentrate of three monomer process wastewater

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Effect test

Embodiment 1

[0045] Embodiment 1 A kind of method for the production of diethylene glycol isophthalate-5-sodium sulfonate from concentrated material of three-monomer process wastewater

[0046] 1. Dissolving and filtering

[0047] Add 600 kg of ethylene glycol to the dissolution kettle, start stirring, and add 400 kg of dried three-monomer production wastewater concentrate to the kettle. To 90°C, keep stirring at this temperature for 65 minutes. Open the discharge valve of the dissolution kettle, feed the centrifuge, centrifuge, and recover the sodium sulfate obtained by the filter cloth to obtain an industrial product that meets the national standard; the obtained filtrate is sucked into the synthesis kettle by vacuum to synthesize SIPE;

[0048] In the dried three-monomer production wastewater concentrate, the moisture content is less than 0.2%, the content of dimethyl-5-sodium isophthalate is 30.02%, and the content of monomethyl-5-sodium isophthalate is The content is 7.35%, and the ...

Embodiment 2

[0066] Embodiment 2 A kind of method for the production of diethylene glycol isophthalate-5-sodium sulfonate from a three-monomer process wastewater concentrate

[0067] Process operation parameter is identical with embodiment 1, and difference is:

[0068] 2. Recovery and treatment of sodium sulfate

[0069] First add 245 kilograms of methanol to the dissolving kettle, start stirring, then add 211 kilograms of sodium sulfate obtained by centrifugation, and all the other operations are the same;

[0070] 3. SIPE synthesis

[0071] The amount of catalyst added is changed to 3000 grams of calcium acetate, 480 grams of dibutyltin oxide, 330 grams of cobalt acetate, and the amount of anti-ether agent added is changed to 240 grams of sodium acetate, and the rest of the operations are the same;

[0072] Judgment of the reaction end point: when the total amount of methanol in the metering methanol receiving tank and the water in the water receiving tank reaches 43.9 kg, it means th...

Embodiment 3

[0077] Embodiment 3 A kind of method for the production of diethylene glycol isophthalate-5-sodium sulfonate from concentrated material of three-monomer process wastewater

[0078] 1. Dissolving and filtering

[0079] Add 550 kg of ethylene glycol to the dissolution kettle, start stirring, and add 370 kilograms of dried three-monomer production wastewater concentrate into the kettle. To 90°C, keep stirring at this temperature for 65 minutes. Open the discharge valve of the dissolution kettle, feed the centrifuge, centrifuge, and recover the sodium sulfate obtained by the filter cloth to obtain an industrial product that meets the national standard; the obtained filtrate is sucked into the synthesis kettle by vacuum to synthesize SIPE;

[0080] This batch of dried three-monomer production wastewater concentrate has a moisture content of less than 0.2%, a content of dimethyl isophthalate-5-sodium sulfonate of 28.33%, monomethyl isophthalate-5-sulfonate The content of sodium su...

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Abstract

The invention provides a method for producing sodium isophthalate-5-sulfonate diethylene glycol ester (SIPE) from the three-monomer process wastewater concentrate, which is characterized in that: the method includes dissolving, filtering, and SIPE synthesis. The SIPE solution prepared by the present invention has low sulfate content, and the sulfate content is 156.48-231.47ppm; the SIPE solution prepared by the present invention has good appearance, high purity, and less impurity content; the appearance is a slightly yellow transparent liquid, and the purity is 94.33-95.1 % (LC), DEG content is 0.12‑0.28%. The reaction temperature of the present invention is low, the reaction temperatures of the first stage and the second stage are respectively 170-180°C and 185-195°C, and the synthesis reaction time is 4.8-5.2h.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for producing diethylene glycol isophthalate-5-sodium sulfonate from a three-monomer process wastewater concentrate. Background technique [0002] Although polyester fiber has the advantages of high modulus, good rigidity, good elasticity, high strength, water resistance, light resistance, good shape retention, and not easy to wrinkle, but due to the lack of energy in polyester macromolecules with direct dyes, acid dyes, and basic dyes Although the functional groups combined with disperse dyes have ester groups that can form hydrogen bonds with disperse dyes, polyester has high crystallinity and compact structure, and it is difficult for dye molecules to enter the interior of the fiber, making dyeing difficult and monotonous in color. For this reason, a strong acidic sulfonic acid group compound can be used to copolymerize with polyester (abbreviated as PET in En...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/58C07C303/32
CPCC07C303/32C07C309/58
Inventor 刘欣杨荣华张秀玲汲彦君刘明明郭祥荣王荣德王璀陈炳瑞倪文龙王建亮
Owner SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI
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