Melamine cardanol modified curing agent preparation method

A technology of melamine and cardanol, used in the chemical industry, climate sustainability, sustainable manufacturing/processing, etc., can solve the problems of severe heat release, excess, and oily surface on the appearance of the paint film, and achieves high reaction temperature and reaction time. fast effect

Active Publication Date: 2019-12-20
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main domestic manufacturers of cardanol curing agent synthesis are: Shanghai Meidong Biomaterials Co., Ltd., Cardolite Zhuhai Co., Ltd., etc., they mainly use cardanol, aldehydes (formaldehyde, paraformaldehyde, paraformaldehyde), polyamines (or mixed amine) carries out Mannich reaction and makes cardanol solidifying agent, exothermic heat is too violent when adding paraformaldehyde to carry out reaction due to one-time addition, and operation risk is very high; Therefore usually adopt the method for adding paraformaldehyde in batches, After the reaction, excess polyamines and aldehydes and the water produced by the reaction have the following defects in this process: the amine compounds (polyamines) are substantially excessive in the reaction process, and when the reaction is completed, the vacuum distillation process is basically Difficult to clean amine compounds (polyamines)
Secondly, when amine compounds (polyamines) use small molecular amines, there are still the following disadvantages: small molecular amines are highly volatile and toxic, and the residual small molecular amine compounds affect the paint film performance of the product, resulting in the appearance of the paint film. There are serious defects such as oily surface and white film
In the process of this preparation method, cardanol, paraformaldehyde, melamine and amine compounds undergo Mannich reaction, and the reaction temperature is 80-90°C. At such a high temperature, a large amount of melamine will undergo its own polymerization side reaction, A large amount of dimer and polymer products are produced, the self-polymerization product of melamine is solid and remains in the product, and the self-polymerization product of melamine is a fine solid, which is difficult to separate from the modified cardanol curing agent product, and filtered After being placed for 3 days, there is still solid precipitation, and there is still solid precipitation at low temperature, and the product after precipitation is turbid. Although there is a melamine curing agent in the modified cardanol, the product is turbid and cannot be applied to the smear layer. There is a large amount of Turbidity, which will affect the surface smoothness of the paint film when applied

Method used

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  • Melamine cardanol modified curing agent preparation method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A preparation method of melamine cardanol modified curing agent, comprising the following steps:

[0033] 1) Add 150 g of cardanol, 30 g of paraformaldehyde and 6 g of melamine into a four-necked flask and mix evenly to obtain a mixture A; add ethylenediamine (30 g) dropwise to the mixture A, exothermic during the addition of ethylenediamine Obviously, control the mixing temperature of the mixture A and the dropwise added ethylenediamine to react at 45-50° C. After the dropwise addition of ethylenediamine is completed (the dropwise addition time is about 1 hour), keep warm and continue to react for 2 hours;

[0034] 2) Step 1) After the heat preservation reaction is completed, add the remaining cardanol 150g and the remaining paraformaldehyde 30g, control the temperature at 45-50°C and add ethylenediamine (30g) dropwise, after the addition of ethylenediamine is completed (dropping time is about 1 hour), insulation continues to react for 1 hour;

[0035] 3) Step 2) Afte...

Embodiment 2

[0040] A preparation method of melamine cardanol modified curing agent, comprising the following steps:

[0041] 1) Add 151 g of cardanol, 31 g of paraformaldehyde and 6 g of melamine into a four-necked flask and mix uniformly to obtain a mixture A; add ethylenediamine (20 g) dropwise to the mixture A, exothermic during the addition of ethylenediamine Obviously, control the mixing temperature of the mixture A and the ethylenediamine added dropwise to react at 40-45° C. After the dropwise addition of ethylenediamine is completed (the dropping time is about 1 hour), keep warm and continue to react for 2 hours;

[0042] 2) Step 1) After the heat preservation reaction, add the remaining cardanol 148g and the remaining paraformaldehyde 30g, control the temperature at 40-45°C and add ethylenediamine (20g) dropwise, after the addition of ethylenediamine is completed (dropping time is about 1 hour), insulation continues to react for 2 hours;

[0043] 3) Step 2) After the heat preserv...

Embodiment 3

[0045] A preparation method of melamine cardanol modified curing agent, comprising the following steps:

[0046] 1) Add 152 g of cardanol, 35 g of paraformaldehyde and 12 g of melamine into a four-necked flask and mix uniformly to obtain a mixture A; add ethylenediamine (20 g) dropwise to the mixture A, exothermic during the addition of ethylenediamine Obviously, control the mixing temperature of the mixture A and the ethylenediamine added dropwise to react at 40-45° C. After the dropwise addition of ethylenediamine is completed (the dropping time is about 1 hour), keep warm and continue to react for 2 hours;

[0047] 2) Step 1) After the heat preservation reaction is completed, add the remaining cardanol 150g and the remaining paraformaldehyde 35g, control the temperature at 40-45°C and add ethylenediamine (20g) dropwise, after the addition of ethylenediamine is completed (dropping time is about 1 hour), insulation continues to react for 2 hours;

[0048] 3) Step 2) After th...

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Abstract

The invention discloses a melamine cardanol modified curing agent preparation method, which comprises: uniformly mixing 140-155 parts of cardanol, 28-40 parts of paraformaldehyde and 5-15 parts of melamine, adding 20-110 parts of an amine compound in a dropwise manner, controlling the temperature at 30-50 DEG C, carrying out a reaction, carrying out thermal insulation after completing the adding,and continuously carrying out a reaction for 1-3 h; adding 140-155 parts of cardanol and 28-40 parts of paraformaldehyde, controlling the temperature at 40-50 DEG C, adding 20-110 parts of an amine compound in a dropwise manner, carrying out thermal insulation after completing the adding, and continuously carrying out a reaction for 1-3 h; adding an organic solvent into the reaction solution, stirring and uniformly mixing, and carrying out thermal insulation standing layering to obtain an upper-layer organic phase and a lower-layer water phase; and carrying out pressure reducing distillation on the obtained upper-layer organic phase to obtain the melamine cardanol modified curing agent. According to the present invention, the prepared modified cardanol curing agent product cannot produce turbidity after being placed for 6 months, the surface smoothness of the paint film cannot be affected during the application of the prepared modified cardanol curing agent product, and the good effectis achieved.

Description

technical field [0001] The invention relates to a preparation method of a melamine cardanol modified curing agent. Background technique [0002] Cardanol is extracted from natural cashew nut shell oil by advanced technology, and can replace or partially replace phenol for the manufacture of epoxy curing agent, liquid phenolic resin, liquid or powdered thermosetting phenolic resin. [0003] At present, my country is a country with a large demand for cardanol, and it is also the most important importer of cashew nut shell liquid in the international market. Due to the renewable nature of cardanol, it has been paid more and more attention, which can save social resources. In the application of cardanol, it is mainly the preparation of cardanol curing agent. The prepared curing agent is cured with epoxy resin at high temperature to obtain a paint film with corrosion resistance, high temperature resistance and good operation at low temperature. The obtained paint The film is mai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/10C08G14/073C08G59/62
CPCC08G14/10C08G14/06C08G59/623Y02P20/10
Inventor 王秋伟牛丽丹金译平
Owner ZHEJIANG WANSHENG
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