Olefin aldehyde condensation reaction method

A technology for condensation reaction and olefinic aldehyde, which is applied in the field of olefinic aldehyde condensation reaction, can solve the problems of lower formaldehyde conversion rate and poor reusability of ionic liquid catalysts, etc., and achieve improved glass transition temperature, good heat resistance, The effect of improving thermal stability

Inactive Publication Date: 2019-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With ionic liquid [BMIM][HSO 4 ] When used as a catalyst, the formaldehyde conversion rate can reach up to 95%, but repeated tests show that the repeated use performance of the ionic liquid catalyst is not good, and after 5 times of use, the formaldehyde conversion rate has been reduced to 90%

Method used

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  • Olefin aldehyde condensation reaction method
  • Olefin aldehyde condensation reaction method
  • Olefin aldehyde condensation reaction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] [Example 1] Preparation of Ion Exchange Resin Catalyst

[0046] Add 47.0 grams of styrene, 2.3 grams of divinylbenzene, 30 grams of polystyrene and 1.6 grams of benzoyl peroxide initiator in a 500 milliliter three-necked flask, stir and react for 1.5 hours at 60 ° C; then add 0.6 grams of multi-walled Carbon nanotubes, continue stirring for 1 hour for pre-polymerization. 260 mL of deionized water in which 2.0 g of gelatin had been dissolved was added. Adjust the stirring speed, and at the same time gradually raise the temperature to 80°C, and react for 5 hours; then raise the temperature to 90°C, react for 5 hours, and finally raise the temperature to 98°C, and react for 8 hours. After the reaction, pour out the upper liquid, wash it with 85°C hot water, then wash it with cold water, then filter, put it in an oven to dry at 80°C, and sieve it to collect composite macropores with a particle size within the range of 0.35-0.60mm. Microsphere A1.

[0047] Chloromethylati...

Embodiment 2

[0052] [Example 2] Preparation of Ion Exchange Resin Catalyst

[0053] Add monomer mixture solution (60.0 gram styrene, 1.0 gram divinylbenzene, 60 gram polystyrene, 1.6 gram multi-walled carbon nanotubes and 1.0 gram benzoyl peroxide containing initiator in 500 milliliters of there-necked flasks, The solution was first stirred and reacted at 70°C for 0.5 hours), started the agitator, added a mixed solution of 200 ml of deionized water and 4 grams of polyvinyl alcohol, raised the temperature to 85°C, reacted for 3 hours, then raised the temperature to 90°C, and reacted for 9 hours , and finally raised the temperature to 100°C, and reacted for 10 hours. After the reaction, pour out the upper liquid, wash with 85°C hot water, then wash with cold water, then filter, put in an oven to dry at 80°C, sieve, and collect composite macropores with a particle size within the range of 0.35 to 0.60 mm Microsphere B1.

[0054] Chloromethylation of composite microspheres: in a 500-ml three...

Embodiment 3

[0059] [Example 3] Preparation of Ion Exchange Resin Catalyst

[0060] Add monomer mixture solution (42.5 gram styrene, 2.5 gram divinylbenzene, 10 gram polystyrene, 0.1 gram multi-walled carbon nanotube and 2.0 gram benzoyl peroxide containing initiator in 500 milliliters of there-necked flasks, The solution was first stirred and reacted at 70°C for 1.5 hours), a mixed solution of 200 ml of deionized water and 4 grams of polyvinyl alcohol was added, the temperature was raised to 85°C, and the reaction was carried out for 3 hours, then the temperature was raised to 90°C, and the reaction was carried out for 9 hours, and finally the temperature was raised to 100°C, react for 10 hours. After the reaction, pour out the upper liquid, wash with 85°C hot water, then wash with cold water, then filter, put in an oven to dry at 80°C, sieve, and collect composite macropores with a particle size within the range of 0.35 to 0.60 mm Microsphere C1.

[0061] Chloromethylation of composite...

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Abstract

The invention relates to an olefin aldehyde condensation reaction method. The method comprises the following steps that under the olefin aldehyde condensation reaction conditions, olefin and formaldehyde are in contact with ion exchange resin catalysts; the ion exchange resin catalysts have a general formula shown in the description, wherein a ball with a P in the middle is a macroporous nanocomposite resin matrix; M- is a negative ion selected from trifluoromethanesulfonate ions, hydrosulfate ions, hydrophosphate ions, tetrafluoroborate ions or hexafluorophosphate ions; POSS is a cage-shapedsilsesquioxane unit; a structure like a pentagon shown in the description is an imidazolium cation unit; R is a connecting group between the POSS unit and the imidazolium cation unit; R is alkylene orarylene.

Description

technical field [0001] The invention relates to a method for alkenal condensation reaction, in particular to a method for preparing 1,3-dihydric alcohol and / or 1,3-dioxane derivatives through alkenal condensation reaction. Background technique [0002] 1,3-Dihydric alcohol has the characteristics of odorless, low toxicity, and good water solubility, and has a wide range of applications in fine chemicals, medicine, and dyes. 1,3-Diols are mainly used as synthetic monomers of polyester and polyurethane, solvents, antifreeze, etc., and are also important pharmaceutical intermediates and organic synthesis intermediates. In particular, 1,3-propanediol is widely used, and its most important application is the preparation of polytrimethylene terephthalate. Polytrimethylene terephthalate is a polyester material with excellent performance, which combines the high performance of polyethylene terephthalate and the ease of processing of polybutylene terephthalate, and has good nylon I...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01J31/08B01J31/06C07C29/38C07C31/20C07D319/06
CPCY02P20/52
Inventor俞峰萍谢同何文军
OwnerCHINA PETROLEUM & CHEM CORP