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Continuous process and device for synthesizing sodium bis(2-hydroxyethyl) 5-sulphonatoisophthalate with high ester exchange rate through catalytic reaction rectification

A bishydroxyethyl isophthalate and catalytic reaction technology, which is applied in the field of modified polyester production, can solve the problem of large changes in heat demand of transesterification reactors, periodic fluctuations in the operation of heat medium systems, and darkening of product appearance, etc. problems, to achieve the effect of low transesterification rate requirements, stable product quality, and improved product quality

Pending Publication Date: 2020-11-17
北京芯友工程技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the traditional SIPE batch process production, the transesterification reactor has the functions of beating and transesterification reaction, the operation cycle is long, the production efficiency is low, and because of the different conditions of beating and transesterification reaction, the heat demand of the transesterification reactor changes greatly. The operation of the heat medium system fluctuates periodically, and the process conditions of each batch of production, such as: reaction time, heating rate, molar ratio of EG and SIPM, catalyst type and dosage, nitrogen replacement conditions, etc., will have a large impact on the transesterification rate. effect, resulting in batch-to-batch variance
If the transesterification rate is too high, SIPE is prone to self-polymerization; if the transesterification rate is too low, there will be more methanol residues, resulting in methanol (MA) bumping and accumulating on the wall of the kettle after the material is added to the high-temperature polymerization system, causing the system to form Black foreign matter, product appearance becomes darker and performance deteriorates

Method used

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  • Continuous process and device for synthesizing sodium bis(2-hydroxyethyl) 5-sulphonatoisophthalate with high ester exchange rate through catalytic reaction rectification

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Effect test

Embodiment 1

[0033] Such as figure 1 Shown, catalytic reaction rectification of the present invention synthesizes the continuous process of high transesterification rate bishydroxyethyl isophthalate-5-sodium sulfonate, and concrete production process is as follows:

[0034] (1) According to the ratio of raw materials, ethylene glycol (EG), dimethyl isophthalate-5-sodium sulfonate (SIPM) is used in a molar ratio of 10:1, and the catalyst (Zn(AC) 2 ) and EG mass ratio (Zn(AC) 2 / EG)=1:500 is continuously put into the beating tank 2 from the material inlet 1, and after mixing evenly, the slurry flows through the material pipeline from the discharge valve at the bottom of the beating tank 2 and is continuously sent into the pre-esterification reaction kettle by the slurry delivery pump 3 4. The pre-transesterification tank 4 maintains a temperature of 170°C and a pressure of 0.1MPa (gauge pressure) to perform a pre-transesterification reaction until the conversion rate of bishydroxyethyl isoph...

Embodiment 2

[0039] Such as figure 1 Shown, a kind of catalytic reaction rectification of the present invention synthesizes the semi-continuous process and the device of high transesterification rate bishydroxyethyl isophthalate-5-sodium sulfonate, and concrete production process is as follows:

[0040] Raw material ratio: ethylene glycol (EG), dimethyl isophthalate-5-sodium sulfonate (SIPM) molar ratio (SIPM / EG) = 1:20, catalyst zinc acetate (Ca(AC) 2 ), ethylene glycol (EG) mass ratio (Ca(AC) 2 / EG)=1:2000; through the feed port 1, it is continuously put into the beating tank 2, and after stirring evenly, the slurry flows through the material pipeline from the discharge valve at the bottom of the beating tank 2, and is continuously sent into the pre-esterification reaction by the slurry delivery pump 3 Kettle 4, and maintain beating tank 2 liquid level; Pre-esterification reactor 4 maintains temperature 230 ℃, keeps reaction pressure 0.5MPa (gauge pressure), residence time 1h, SIPE conv...

Embodiment 3

[0042] 1. Put 1000.0kg ethylene glycol (EG) into the beating tank 2, 5.0kg manganese acetate (Mn(AC) 2 ), 448.2kg dimethyl isophthalate-5-sodium sulfonate (SIPM), after being stirred evenly, is sent into the pre-esterification reaction kettle 4 continuously by the slurry delivery pump 3 with 145kg / h, and in good time to the beating tank 2 Feed again to maintain the liquid level of the beating tank 2 within a certain range.

[0043] 2. The temperature of the pre-transesterification reactor 4 is stabilized at 190°C, the pressure is controlled at 0.2MPa (gauge pressure), the residence time of the material is 2h, and the product is continuously pumped into the final transesterification reaction by the pre-transesterification material delivery pump 6 at 139.2kg / h Rectifying tower 7; After the methanol produced by transesterification in the pre-transesterification reactor 4 is separated by the methanol fractionation tower 5, the crude methanol is extracted at the top of the tower at...

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Abstract

The invention discloses a continuous process and device for synthesizing sodium bis(2-hydroxyethyl) 5-sulphonatoisophthalate with a high ester exchange rate through catalytic reaction rectification. Materials are subjected to pre-transesterification through a full-mixing reaction kettle and then enter a final transesterification reaction rectifying tower, so a transesterification rate is further improved; a sodium bis(2-hydroxyethyl) 5-sulphonatoisophthalate solution continuously extracted from the bottom of the reaction rectifying tower is fed into a product blending tank; ethylene glycol isadded for blending to obtain an end product, and the end product is sent to a finished product tank to obtain a final product. The device comprises a pulping tank, the pre-transesterification reactionkettle, a final transesterification reaction rectifying tower, a product blending tank and the finished product tank, wherein a condensing tower is arranged at the top of the pre-transesterificationreaction kettle; a condenser is arranged at the top of the final transesterification rectifying tower; and the condensing tower at the top of the pre-transesterification reaction kettle and the condenser at the top of the final transesterification reaction rectifying tower are connected with a methanol tank. The sodium bis(2-hydroxyethyl) 5-sulphonatoisophthalate produced by the method has the advantages of high ester exchange rate, reduced side reaction and stable product quality.

Description

technical field [0001] The invention belongs to the technical field of modified polyester production, and relates to a two-stage transesterification reaction between ethylene glycol (EG) and dimethyl isophthalate-5-sodium sulfonate (SIPM) under catalytic reaction rectification conditions The continuous process method adopts a two-stage continuous transesterification process to synthesize the production process and device of bishydroxyethyl isophthalate-5-sodium sulfonate (SIPE) with high transesterification rate. Background technique [0002] Polyester is difficult to dye, and the preparation of cationic dye-dyeable polyester is one of the important ways to solve the difficulty of polyester dyeing. Bishydroxyethyl isophthalate-5-sodium sulfonate (SIPE) is a polyester dyeing modifier, which is added as the third monomer of the reaction. Because the modified polyester contains sulfonic acid groups, it has good affinity for cationic dyes. After dyeing, the fiber has bright col...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C303/44C07C309/58
CPCC07C303/32C07C303/44C07C309/58
Inventor 李传迎虞小三屈超
Owner 北京芯友工程技术有限公司
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