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A kind of refining method for removing trace aldehyde group in 1,3-propanediol

A purification method and technology of propylene glycol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of slow reaction rate, high resin cost, poor effect, etc., and achieve easy separation, simple operation, and low cost. Obvious effect

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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AI Technical Summary

Problems solved by technology

[0008] 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 dealdehyde effect is good, but the resin itself has the disadvantages of high cost, slow reaction rate, and poor thermal stability. , non-renewable and other shortcomings
[0009] Therefore, in view of the problem of high aldehyde-based impurities in the 1,3-PDO product existing in the above-mentioned acrolein hydration hydrogenation process, it is necessary to find a more effective method to solve the deficiencies in the prior art

Method used

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  • A kind of refining method for removing trace aldehyde group in 1,3-propanediol
  • A kind of refining method for removing trace aldehyde group in 1,3-propanediol
  • A kind of refining method for removing trace aldehyde group in 1,3-propanediol

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Embodiment 1-16

[0059] Preheat the 1,3-propanediol solution containing aldehyde-based impurities to 60-140°C, pump 250 mL into a stirred tank reactor, add sulfonic acid ionic liquid to a concentration of 0.1-10wt%, and carry out dealdehyde reaction , the reaction time is 0.5-6h. The treated 1,3-propanediol is distilled, the number of column plates is 16-40, the temperature of the column kettle is 138-155°C, the reflux ratio is 2:1-15:1, and the pressure at the top of the column is 1-10kPa. The specific operating conditions and treatment effects are shown in the following table, and the aldehyde group content in the raw material before the dealdehyde treatment is 792 ppm.

[0060] Table 1 Dealdehyde technology and effect of different sulfonic acid ionic liquids

[0061]

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Abstract

The invention relates to a method for removing residual trace impurities containing aldehyde groups in 1,3-propylene glycol (1,3-PDO). The 1,3-PDO solution obtained after the 3-hydroxypropionaldehyde hydrogenation reaction product is dehydrated and concentrated contains a trace amount of aldehyde group impurity, and the sulfonic acid ionic liquid is added to the solution, and the dealdehyde treatment is carried out at a certain temperature, The 1,3-PDO solution after aldehyde removal by rectification under vacuum, and the distillate is condensed to obtain a high-purity 1,3-PDO product. The 1,3-PDO produced by the acrolein hydration route can reduce the residual aldehyde impurity content to less than 10 ppm after adopting this method, and obtain a product with a purity higher than 99.7%, which meets the requirements for the quality of raw materials in the synthesis of low-color polyester PTT. Require. The treatment method is simple to operate, green and efficient, and the acidic ionic liquid can be recycled.

Description

technical field [0001] The invention belongs to the field of purification and purification of chemical synthesis, in particular to a purification method for removing trace aldehyde groups in 1,3-propanediol. Background technique [0002] 1,3-Propanediol (1,3-PDO) is an important organic chemical raw material, which is widely used in organic solvents, lubricants, antifreezes, pharmaceutical intermediates, cosmetics, synthesis of heterocyclic compounds and other fields. , 1,3-PDO also has broad application prospects in thermoplastic polyurethane, copolyester and engineering plastics. At present, its main application is to synthesize a new type of polyester material-polytrimethylene terephthalate (PTT) as a polymerized monomer. [0003] Since the advent of polyethylene terephthalate (PET) fiber, it has been leading the development trend of synthetic fiber. PTT has both the high strength and stability of PET and the excellent molding and processing type of PBT (polybutylene ter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/20C07C29/88C07C29/80B01J31/02
CPCC07C29/88C07C29/80B01J31/0284C07C31/205
Inventor 赵聪袁帅王中华黄少峰刘振峰
Owner WANHUA CHEM GRP CO LTD
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