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The scale-up preparation method, production equipment and stability evaluation method of special phenolic resin with narrow distribution and wide processing window

A technology of phenolic resin and formaldehyde, which is applied in the field of phenolic resin preparation, can solve the problems of many active sites, high reactivity, complex resin structure, composition and reaction route, etc., to ensure uniformity, improve mixing effect, and ensure measurement The effect of warm accuracy

Active Publication Date: 2022-02-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, high reactivity, many active sites, and diversified reaction pathways lead to phenolic resins becoming a mixture of components with different degrees of polymerization, different isomers, and different functional group contents.
For example, for thermosetting phenolic resins, there are both methylene bridge structures and high content of methylol groups in the molecular structure of the resin, where methylene groups can be connected at the ortho or para positions of the phenolic rings, each The position and number of methylol functional groups connected to each phenol ring are different, and may also contain a small amount of methylene ether structure, so the structure, composition and reaction route of the resin are very complicated

Method used

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  • The scale-up preparation method, production equipment and stability evaluation method of special phenolic resin with narrow distribution and wide processing window
  • The scale-up preparation method, production equipment and stability evaluation method of special phenolic resin with narrow distribution and wide processing window
  • The scale-up preparation method, production equipment and stability evaluation method of special phenolic resin with narrow distribution and wide processing window

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Experimental program
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preparation example Construction

[0100] As mentioned above, the present invention provides a method for stably preparing special phenolic resin with narrow distribution and wide processing window, which includes the following steps:

[0101] Step 1. Special phenolic resin addition and condensation reaction stage: control the preheating temperature of the raw material phenol in the feeding stage at 55±1°C, pump the phenol into the addition condensation reaction device through vacuum, and pump the formaldehyde into the metering tank; heat the phenol to 65±1°C, add catalyst and keep it warm for 30 minutes to keep the temperature of the material constant, start adding formaldehyde dropwise, complete the dropwise addition of formaldehyde within 60±5 minutes, and then raise the material to 90±1°C within 40±5 minutes , the heat preservation reaction is about 3 hours, the refractive index is 1.5250-1.5370, and the addition condensation reaction is completed;

[0102] Step 2, neutralization reaction stage: After the a...

Embodiment A-1

[0109] Addition condensation reaction device for the expansion of special phenolic resins, such as figure 1 As shown, it includes a kettle body, an online viscometer, a temperature control unit (TCU) 8, a temperature measuring point 6, a stirring mechanism and a vacuum unit 7.

[0110] The volume of the kettle body is 3m 3 , the top of the kettle body is provided with a feeding port, the feeding port is connected with the formaldehyde dripping tank 9, the kettle body adopts the temperature control mode of inner coil pipe 3 heating, reactor jacket cooling, valve switch switchable, to improve the heating and cooling of materials efficiency.

[0111] The stirring mechanism of the addition condensation reaction device is a three-layer frame stirring 4, which can improve the mixing effect of the materials and the uniformity of the temperature of the materials.

[0112] The addition condensation reaction device adopts "upper-middle-lower" three-point temperature measurement, and t...

Embodiment A-2

[0117] The production system for the expansion preparation of special phenolic resins includes the addition condensation reaction device, filter mechanism, metering tank and feeding tank in Example A-1, and an optional independent dehydration reaction kettle. The structure of the independent dehydration reaction tank is the same as that of the addition condensation reaction device. The filtering mechanism is arranged outside the addition-condensation reaction kettle, and is used for filtering the reaction materials obtained in the neutralization reaction stage. After the reaction material obtained in the neutralization reaction stage is filtered by the filter mechanism, it can be returned to the addition condensation reaction kettle for dehydration reaction. At this time, the addition condensation reaction kettle becomes a dehydration reaction kettle; or enters an independently set dehydration reaction kettle .

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Abstract

The invention discloses an expansion preparation method, production device and stability evaluation method of special phenolic resin with narrow distribution and wide processing window, belonging to the field of high-end phenolic resin manufacturing. The expansion preparation method of the present invention clarifies the characteristics of the key process parameters in the resin preparation process, and strengthens the overall process and end point control of the synthesis reaction from the three key links of the addition condensation reaction stage, neutralization reaction stage and dehydration reaction stage , which ensures the smoothness, stability and reproducibility of the resin preparation process. The evaluation method of the resin quality stability provided by the invention is used to evaluate the quality and performance stability of the resin by testing the intrinsic structure of the resin combined with the physical and chemical indicators of the resin. The production device provided by the invention provides guarantee for the uniformity of materials, the stability of heat history and the real-time performance of process control in the whole process of resin preparation, and ensures the stability of the quality and performance of the prepared phenolic resin.

Description

technical field [0001] The invention belongs to the field of preparation of phenolic resins, relates to a method for preparing high-end phenolic resins and evaluating their stability, and in particular to a preparation method for the expansion of special phenolic resins with a narrow distribution and a wide processing window, a production device and an evaluation of their stability method. Background technique [0002] Phenolic resin is one of the earliest synthetic polymer materials recognized by humans. It is prepared by the polycondensation reaction between phenol and formaldehyde. The reactivity between phenol and formaldehyde is relatively high, and under the catalysis of acid or alkali, the reaction can be carried out quickly by heating, so the phenolic resin is relatively easy to synthesize. However, high reactivity, many active sites, and diversified reaction pathways lead to phenolic resins becoming a mixture of components with different degrees of polymerization, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10G01N33/44B01J3/00B01J19/00B01J19/18
CPCC08G8/10G01N33/442B01J3/006B01J3/002B01J19/1862B01J19/0053B01J19/0006B01J19/0013B01J2219/00063B01J2219/00081B01J2219/00162
Inventor 赵彤罗振华郭文强杜有培田昶斌李昊
Owner INST OF CHEM CHINESE ACAD OF SCI
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