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Preparation method of THEIC modified melamine formaldehyde resin

The technology of melamine and formaldehyde resin is applied in the fields of chemical industry and polymer material auxiliaries, which can solve the problems of difficulty in coloring, waste water containing sodium chloride, large solvent loss, etc. Simple, no three wastes discharge effect

Active Publication Date: 2021-03-09
QINGDAO UNIV OF SCI & TECH
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AI Technical Summary

Problems solved by technology

Nevertheless, this type of char-forming agent also has the following problems: 1) It mainly uses cyanuric chloride, unit amines (such as ethanolamine, butylamine, etc.) and polyamines (such as ethylenediamine, piperazine) as raw materials , prepared by condensation and polycondensation
Due to the incomplete replacement of cyanuric chloride, the product generally contains about 1.0% chlorine, which cannot fully meet the user's halogen-free requirements for flame retardants, and there are still certain safety problems; 2) A large amount of chlorine-containing chlorine is produced during the production process Sodium wastewater, difficult to treat
In addition, due to the use of a large amount of low boiling point solvents (such as acetone) in the production process, the solvent loss is large, causing serious air pollution; 3) the flame retardant effect and water resistance need to be further improved, and the flame retardant The water resistance of the material still cannot meet the quality standards at home and abroad
[0005] Tris (2-hydroxyethyl) isocyanurate (abbreviated as Saike or THEIC) is an easy-to-synthesize, inexpensive small-molecule triazine compound, which also has a good char-forming effect [Li Yongqiang, Hao Qiufen, Yang Jingwei, et al. .Study on the Synergistic Flame Retardant Effect of Type II Ammonium Polyphosphate and Sekke on Polypropylene, Qingdao University of Science and Technology (Natural Science Edition), 2013,34(3):231-235,240; Wenyan Chen, Shanshan Yuan, Yong Sheng, et al .Effect of Charring Agent THEIC onFlame Retardant Properties of Polypropylene, J.APPL.POLYM.SCI.,2015:41214(1-8)], but it is easily soluble in water, easy to migrate and precipitate
Since N-CH 2 The high OH activity leads to the unsatisfactory thermal stability of Saike modified melamine formaldehyde resin, and it is prone to yellowing when heated, resulting in yellowing of flame retardant products, making it difficult to color, and releasing a small amount of toxic Gas - formaldehyde

Method used

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Examples

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preparation example Construction

[0024] Preparation of flame retardant PP samples: Extrude PP and IFR in a twin-screw extruder (rotating speed 20-30rpm) at 190-200°C at a mass ratio of 70:30, mix and granulate. The dried granules are molded with a tablet press at 200-210°C under a pressure of 5MPa, then cold-pressed under a pressure of 5MPa, and then cut into strips of required specifications for performance testing.

[0025] Flame retardant performance test: vertical combustion test adopts CZF-3 horizontal and vertical combustion tester (Nanjing Jiangning District Analytical Instrument Factory) referring to GB / T2408-1996 test, and the sample size is 100mm×13mm×1.6mm.

[0026] The polypropylene used in this application (abbreviated as PP) is the PPSP179 type copolymerized polypropylene produced by China Petroleum & Chemical Co., Ltd. Qilu Branch and the PPH8020 homopolymerized polypropylene produced by Lanzhou Petrochemical Company of China Petroleum and Natural Gas Co., Ltd., both by mass ratio w (PP SP179):...

Embodiment 1

[0028] The preparation process of Saike modified melamine formaldehyde resin, the specific steps are as follows:

[0029] First add 1 kg of hexamethoxymethyl melamine and 1.68 kg of sek to the kneader with heating device, start stirring and heat until sek is completely melted, then add 0.025 kg of p-toluenesulfonic acid, and heat the material to 150± React at 5°C for 4 hours, then cool to room temperature, pour the material out of the kneader, and pulverize it into a powder product with a pulverizer. The obtained product has a quality of 2.12kg, a mass yield of 79.1%, and a water solubility of 0.15g / 100mL of water. Product weight loss 2% (T 2wt％ ), 5% (T5wt％ ), 10% (T 10wt％ ) temperature and the temperature T at the time of maximum thermogravimetric loss max They are 267°C, 298°C, 323°C and 345°C, respectively.

[0030] In the present invention, the structure of the product obtained in this embodiment is characterized by infrared spectroscopy and carbon nuclear magnetic re...

Embodiment 2

[0035] The preparation process of Saike modified melamine formaldehyde resin, the specific steps are as follows:

[0036] First, add 1 kg of hexamethoxymethylmelamine and 2.00 kg of Sek into the kneader with a heating device, start stirring and heat until the Sek is completely melted, then add 0.026 kg of p-toluenesulfonic acid, and heat the material to 150± React at 5°C for 4 hours, then cool to room temperature, pour the material out of the kneader, and pulverize it into a powder product with a pulverizer. The obtained product has a quality of 2.42kg, a mass yield of 80.7%, and a water solubility of 0.32g / 100mL of water. Product weight loss 2% (T 2wt％ ), 5% (T 5wt％ ), 10% (T 10wt％ ) temperature and the temperature T at the time of maximum thermogravimetric loss max They are 263°C, 296°C, 320°C and 341°C, respectively.

[0037] The product of this example was detected according to the characterization method in Example 1, and it was proved that the product obtained in th...

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Abstract

The invention discloses a preparation method of a THEIC modified melamine formaldehyde resin. The resin is prepared through solvent-free ether exchange by taking hexamethoxymethyl melamine and THEIC as raw materials and p-toluene sulfonic acid as a catalyst. The preparation method comprises the following specific steps: adding hexamethoxymethyl melamine and THEIC into a kneading machine with a heating device, starting stirring, heating until THEIC is completely molten, adding p-toluene sulfonic acid, heating the materials to 110-180 DEG C, reacting for 1-8 hours, cooling to room temperature, pouring out the materials from the kneading machine, and pulverizing into a powder product by using a pulverizer. The resin has the advantages that the preparation process is simple, basically no threewastes are discharged in the preparation process, and the product is low in water solubility, good in heat resistance and char forming property, not prone to yellowing when heated and free of formaldehyde release.

Description

technical field [0001] What the present invention relates to is a kind of preparation method of melamine formaldehyde resin modified by SEC, specifically using hexamethoxymethyl melamine and SEC as raw materials, p-toluenesulfonic acid as catalyst, and producing SEC by solvent-free ether exchange The invention discloses a method for modifying melamine-formaldehyde resin, which belongs to the field of chemicals and polymer material additives. Background technique [0002] Intumescent flame retardant (IFR) is a kind of composite flame retardant system composed of acid source (dehydrating agent), carbon source (char forming agent) and gas source (foaming agent). It has high flame retardant efficiency, It has the advantages of low smoke and low toxicity of the gas released during combustion, which meets the requirements of current flame retardant materials for smoke suppression and environmental protection [Tang Shuo, Jin Yujuan, Qian Lijun. Research progress of intumescent flam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/42
CPCC08G12/427
Inventor 何为孙明媚颜博陈程刘文昊王政文唐林生
Owner QINGDAO UNIV OF SCI & TECH
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