Method for removing micro aldehyde group from 1,3-propylene glycol

A technology for removing propylene glycol, which is applied in 1 field, can solve problems such as poor effect, high resin cost, and slow reaction rate, and achieve good effect of dealdehyde removal and low cost

Active Publication Date: 2006-07-19
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above method, the effect of dealdehydeization is poor when using clay and ammonia derivatives, and when acid-base ion exchange resin is used as a catalyst, the...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation of SO by impregnation 4 2- / ZrO 2 -Al 2 o 3 Solid super acid. Weigh 250.2gAl(NO 3 ) 3 9H 2 O and 70.8 g ZrOCl 2 ·8H 2 O (the atomic ratio of Al and Zr is 3) is placed in a 1000ml three-neck round bottom flask, and 466ml of deionized water is added under stirring conditions to fully dissolve, and then concentrated ammonia water is slowly added dropwise to adjust the pH value of the solution to 8-9, and the precipitation is complete. , Aging for 24h, suction filtration to obtain a white precipitate. Dry the precipitate at 110°C for 12 hours, grind it finely, then weigh 30g and put it into a 800ml beaker, add 450ml of 0.5mol / L H 2 SO 4 The solution was soaked for 8 hours, filtered, washed and dried, then calcined at 650°C for 3 hours to obtain SO 4 2- / ZrO 2 -A 2 o 3 Catalyst (referred to as Catalyst A).

[0014] 250g of 1,3-propanediol dehydration concentrate (1,3-propanediol weight percentage is about 78%) and 25g of catalyst A are placed in ...

Embodiment 2

[0016] Preparation of SO by impregnation 4 2- / ZrO 2 -SiO 2 Solid super acid. Weigh 280.3gNa respectively 2 SiO 3 9H 2 O and 102.1 g ZrOCl 2 ·8H 2 O (the atomic ratio of Si and Zr is 3) is placed in a 1000ml three-necked round bottom flask, and 550ml of deionized water is added under stirring conditions to fully dissolve, and then concentrated ammonia water is slowly added dropwise to adjust the pH of the solution to 8-9, and the precipitation is complete. , Aging for 24h, suction filtration to obtain a white precipitate. Dry the precipitate at 110°C for 12 hours, grind it finely, then weigh 30g and put it into a 800ml beaker, add 450ml of 0.5mol / L H 2 SO 4 The solution was soaked for 8 hours, filtered, washed and dried, then calcined at 650°C for 3 hours to obtain SO 4 2- / ZrO 2 -SiO 2 Catalyst (referred to as Catalyst B).

[0017] Catalyst B was used to carry out dealdehyde reaction and 1,3-propanediol rectification purification under the same conditions as in...

Embodiment 3

[0019] Preparation of SO by impregnation 4 2- / SnO 2 -Al 2 o 3 Solid super acid. Weigh 250.2gAl(NO 3 ) 3 9H 2 O and 57.3 g SnCl 4 (Al and Sn atomic ratio is 3) placed in a 1000ml three-neck round-bottomed flask, under stirring conditions, add 550ml deionized water to fully dissolve, then slowly add concentrated ammonia water to adjust the pH value of the solution to 8-9, and let stand after the precipitation is complete. After aging for 24 hours, a white precipitate was obtained by suction filtration. Dry the precipitate at 110°C for 12 hours, grind it finely, then weigh 30g and put it into a 800ml beaker, add 450ml of 0.5mol / L H 2 SO 4 Soak in aqueous solution for 8 hours, filter, wash, and dry, then roast at 550°C for 3 hours to obtain SO 4 2- / SnO 2 -Al 2 o 3 Catalyst (referred to as Catalyst C).

[0020] Catalyst C was used to carry out dealdehyde reaction and 1,3-propanediol distillation and purification under the same conditions as in Example 1. See Tabl...

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Abstract

The related stripping method for trace-amount aldehydo in 1, 3-dihydroxypropane comprises: adding proper solid super acidic catalyst of SO42-/MxOy into the 1, 3-dihydroxypropane solution with micro impurity dewatered and condensed from hydrogenation reaction production of 3-hydroxypropionaldehyde for dealdehydation treatment at given temperature; rectifying the solution under vacuum to obtain polymer-grade product that has 1, 3-dihydroxypropane content more than 99.7% and aldehyde content less than 10ppm and fit to material quality request for PTT.

Description

technical field [0001] The invention relates to a method for refining and purifying 1,3-propanediol, especially a method for removing trace aldehyde groups in 1,3-propanediol. Background technique [0002] 1,3-propanediol is an important new organic chemical raw material, which can be used as a monomer for the synthesis of polyester and polyurethane. Polyethylene terephthalate (PTT) synthesized with 1,3-propanediol as a monomer has better performance than polyethylene terephthalate (PET) synthesized with ethylene glycol. PTT fiber not only has the performance of PET, but also has good resilience and anti-pollution performance of nylon. However, due to the high price of 1,3-propanediol, the high production cost of PTT limits its market competition with PET. Since Degussa and Shell successively achieved large-scale industrial production of 1,3-propanediol in the 1990s, the good development prospects of PTT have gradually attracted widespread attention. [0003] When acrolei...

Claims

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Application Information

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IPC IPC(8): C07C29/74C07C31/20B01J27/053
Inventor 原宇航张春雷赵志宏崔曜邵敬铭
Owner SHANGHAI HUAYI NEW MATERIAL
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