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Modified resin catalyst and method for removing residual formaldehyde in 3-methyl-3-butene-1-ol solution

A technology for modifying resins and catalysts, used in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc. Incomplete, product loss and other problems, to achieve good formaldehyde removal effect, reduce catalyst loss, reduce equipment investment and operation effect

Active Publication Date: 2020-08-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the urea-formaldehyde resin solids produced in this scheme make it difficult for subsequent continuous production and separation, and the formaldehyde treatment is not thorough, and ≥300ppm will remain
[0006] U.S. patent application US6242655B1 discloses a method for removing residual formaldehyde in ethylene glycol solution with a strongly acidic cationic resin. The reaction temperature is 30-50°C, and the formaldehyde content is reduced from 2000ppm to below 100ppm, but the strongly acidic cationic resin will cause 3-methyl - Dehydration of 3-buten-1-ol to isoprene leading to product loss

Method used

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  • Modified resin catalyst and method for removing residual formaldehyde in 3-methyl-3-butene-1-ol solution
  • Modified resin catalyst and method for removing residual formaldehyde in 3-methyl-3-butene-1-ol solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of modified resin catalyst:

[0042] Take 200g of polystyrene-divinylbenzene crosslinking resin (hereinafter referred to as "crosslinking resin") and add it to the chloroform solution, add 0.5wt% graphene oxide of the mass of the crosslinking resin, mix it with ultrasound for 1 hour, and then heat to remove the solvent; The resin was washed three times with ethanol, and then washed with 50 wt % sodium hydroxide aqueous solution until the pH was greater than 10, and finally the resin was put into an oven at 160° C. for 10 h to obtain a modified resin. Add the modified resin to a 2000ml three-necked bottle with a condenser, protect it with nitrogen, and then add 600ml of toluene to soak for 6h; start stirring, and add 2wt% triethylaluminum and 0.3wt% aluminum acetylacetonate (both based on cross-linked resin mass), heated to 120°C and stirred for 3 hours, then lowered the temperature, cooled and filtered to obtain a modified resin catalyst, washed with ethanol...

Embodiment 2

[0046] Preparation of modified resin catalyst:

[0047] Take 200g of polystyrene-divinylbenzene crosslinking resin and add it to the chloroform solution, add 0.5wt% graphene oxide of the mass of the crosslinking resin, mix with ultrasound for 1h, and then heat to remove the solvent; wash the resin 3 times with ethanol, and then use 50wt% The sodium hydroxide aqueous solution was washed until the pH was greater than 10, and finally the resin was dried in an oven at 160° C. for 10 hours to obtain a modified resin. Add the modified resin into a 2000ml there-necked bottle with a condenser and protect it with nitrogen, then add 600ml of toluene and soak for 6h; start stirring, add 4wt% butyllithium and 0.8wt% rhodium acetylacetonate (both based on crosslinked resin mass), heated to 110°C and stirred for 4h, then cooled down and filtered to obtain a modified resin catalyst, washed with ethanol for 3 times, and then dried in a 180°C oven for 24h. In the prepared modified resin catal...

Embodiment 3

[0051] Preparation of modified resin catalyst:

[0052] Take 200g of polystyrene-divinylbenzene crosslinking resin and add it to the chloroform solution, add 0.5wt% graphene oxide of the mass of the crosslinking resin, mix with ultrasound for 1h, and then heat to remove the solvent; wash the resin 3 times with ethanol, and then use 50wt% The sodium hydroxide aqueous solution was washed until the pH was greater than 10, and finally the resin was dried in an oven at 160° C. for 10 hours to obtain a modified resin. Add the modified resin into a 2000ml there-necked bottle with a condenser and protect it with nitrogen, then add 600ml of toluene and soak for 6h; start stirring, add 6wt% dimethyllithium and 1.5wt% magnesium acetylacetonate (based on the quality of the cross-linked resin ), heated to 120° C. and stirred for 3 h, then lowered the temperature, cooled and filtered to obtain a modified resin catalyst, washed the obtained modified resin catalyst with ethanol three times, a...

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Abstract

The invention provides a modified resin catalyst and a method for removing residual formaldehyde in a 3-methyl-3-butene-1-alcohol solution. The modified resin catalyst provided by the invention uses polystyrene-divinylbenzene The resin is a carrier, and the organic metal compound is loaded on the carrier, and the organic metal compound includes an alkyl metal compound. Utilizing the modified resin catalyst of the present invention to remove residual formaldehyde in 3-methyl-3-butene-1-alcohol solution can remove formaldehyde more thoroughly.

Description

technical field [0001] The invention relates to a method for removing residual formaldehyde in 3-methyl-3-butene-1-alcohol solution, in particular to a modified resin catalyst and the use of the modified resin catalyst to remove 3-methyl-3-butane Method for residual formaldehyde in en-1-ol solution. Background technique [0002] 3-Methyl-3-buten-1-ol, mainly used in large-scale production of solvents, dyes, surface coatings, pigments, pesticides and insecticides, etc., one of its new uses is for the new generation of polycarboxylic acid series Preparation of high-efficiency water reducer. On the other hand, isopentenol can be produced by isomerization reaction, and the latter is used as the basic raw material for the production of high-efficiency and low-toxicity pesticides inhibiting pyrethroids and citral series flavors and fragrances. [0003] The existing technical route for synthesizing 3-methyl-3-buten-1-ol is difficult to convert 100% formaldehyde. For example, in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/12B01J31/22C07C29/88C07C29/76C07C33/025
CPCB01J31/12B01J31/143B01J31/2208B01J31/2213B01J2531/22B01J2531/31B01J2531/822B01J2531/842C07C29/76C07C29/88C07C33/025
Inventor 庞计昌刘英俊于斌成朱小瑞张永振姜庆梅黎源
Owner WANHUA CHEM GRP CO LTD
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