Micro-reaction device and method for preparing xylene formaldehyde resin by using micro-reaction device

A technology of xylene formaldehyde resin and micro-reaction device, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical processes, etc. Performance can not meet the requirements, mass transfer and heat transfer efficiency limitations, etc., to achieve the effect of reducing the influence of equipment and operators, increasing the utilization rate of sulfuric acid, and shortening the reaction time

Inactive Publication Date: 2020-03-27
NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the reaction is a two-phase reaction, the mass transfer and heat transfer efficiency of the traditional process is limited in large-scale production. The reaction catalyst is sulfuric acid, and the amount of sulfuric acid greatly affects the discharge of reaction waste acid water.
At the same time, the formaldehyde solution is very volatile during the heating process of more than 100 degrees, which will cause more or less impact on equipment, air and operators, reduce the utilization rate of formaldehyde and lead to low resin yield and unsatisfactory product performance. to request

Method used

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  • Micro-reaction device and method for preparing xylene formaldehyde resin by using micro-reaction device
  • Micro-reaction device and method for preparing xylene formaldehyde resin by using micro-reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The formaldehyde solution (the concentration of the formaldehyde solution is 37wt%) is flushed into the syringe pump as one phase, and the catalyst sulfuric acid (the concentration of sulfuric acid is 92.5wt%) is flushed into the syringe pump as the other phase, and the two phases are simultaneously injected into the first microreactor , heated at 80°C, wherein the molar ratio of formaldehyde to catalyst sulfuric acid is 1:0.15, and the two-phase flow rates are 0.316ml / min and 0.035ml / min respectively; the reaction mixture of formaldehyde and catalyst, and xylene as the other phase The mixture passes through the second microreactor equipped with a backpressure valve at the end, the rated pressure set by the backpressure valve is 15bar, the flow rate of xylene is 0.617ml / min, the second microreactor is placed in an ultrasonic device for ultrasonication, and simultaneously Heat treatment and react at 105°C for 15 minutes, wherein the molar ratio of formaldehyde to xylene i...

Embodiment 2

[0031]The formaldehyde solution (the concentration of the formaldehyde solution is 37wt%) is flushed into the syringe pump as one phase, and the catalyst sulfuric acid (the concentration of sulfuric acid is 90wt%) is flushed into the syringe pump as the other phase, and the two phases are simultaneously injected into the first microreactor, Heating at 80°C, wherein the molar ratio of formaldehyde to catalyst sulfuric acid is 1:0.1, and the two-phase flow rates are 0.318ml / min and 0.024ml / min respectively; the reaction mixture of formaldehyde and catalyst is mixed with xylene as the other phase Through the second microreactor with a backpressure valve at the end, the rated pressure set by the backpressure valve is 13bar, and the xylene flow rate is 0.658ml / min. The second microreactor is placed in an ultrasonic device for ultrasonication and heating Treatment, react at 110°C for 10 minutes, wherein the molar ratio of formaldehyde to xylene is 1:1.27, and the molar ratio of xylen...

Embodiment 3

[0033] The formaldehyde solution (the concentration of the formaldehyde solution is 37wt%) is flushed into the syringe pump as one phase, and the catalyst sulfuric acid (the concentration of sulfuric acid is 95wt%) is flushed into the syringe pump as the other phase, and the two phases are simultaneously injected into the first microreactor, Heating at 80°C, wherein the molar ratio of formaldehyde to catalyst sulfuric acid is 1:0.2, and the two-phase flow rates are 0.312ml / min and 0.045ml / min respectively; the reaction mixture of formaldehyde and catalyst is mixed with xylene as the other phase Through the second microreactor with a back pressure valve at the end, the rated pressure set by the back pressure valve is 10bar, the flow rate of xylene is 0.643ml / min, the second microreactor is placed in an ultrasonic device for ultrasonication and heating Treatment, react at 120°C for 15 minutes, wherein the molar ratio of formaldehyde to xylene is 1:1.27, and the molar ratio of xyl...

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Abstract

The invention provides a micro-reaction device and a method for preparing xylene formaldehyde resin. The method comprises the following steps: simultaneously pumping a formaldehyde aqueous solution and a catalyst aqueous solution into a first mixer of the micro-reaction device for mixing, then generating a reaction product in a first micro-reactor, mixing the reaction product with xylene in a second mixer, carrying out ultrasonic treatment and heating reaction in a second micro-reactor, carrying out water washing or alkali washing to remove a water layer and then carrying out rotary evaporation to obtain the product. Compared with the existing preparation method, the method has the advantages that the use amount of sulfuric acid is greatly reduced and corrosion to equipment and pollution of reaction waste liquid to the environment are reduced; the formaldehyde solution and the xylene are subjected to ultrasonic treatment and can be sufficiently emulsified to form microemulsion so thattwo-phase reaction raw materials are in more sufficient contact and the mass and heat transfer efficiency is greatly improved; meanwhile, the reaction system can bear certain pressure so that volatilization of the formaldehyde solution is reduced, the utilization rate of the formaldehyde is greatly increased and the product yield can be increased by 30%-40% relative to that in a reaction kettle.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a micro-reaction device and a method for preparing xylene formaldehyde resin by using the same. Background technique [0002] At present, xylene formaldehyde resin has been widely used, and can be used as a modifier for polymer plasticizers, synthetic resins, and synthetic materials. Xylene formaldehyde resin has excellent acid and alkali resistance, and can be used to modify phenolic resins. The more, the more corrosion resistant. At the same time, it can also undergo a series of modifications, and the modified resin is widely used in industries such as industrial rubber, artificial leather and glass fiber reinforced plastics. [0003] In the existing xylene-formaldehyde resin preparation process, formaldehyde solution and xylene react for 12 hours under the condition of sulfuric acid as a catalyst for polymerization, and after post-treatment, a yellow viscous polymer is gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C08G10/02
CPCB01J19/0093C08G10/02
Inventor 郭凯何伟李玉光沈磊李亚军
Owner NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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