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THEIC derivative and preparation method thereof

A derivative and polyester technology, applied in the field of chemical and polymer material additives, can solve the problems of reduced carbon-forming performance, poor compatibility, easy to turn yellow, etc., and achieve good carbon-forming properties and thermal stability, The preparation process is simple and the effect of no three wastes discharge

Active Publication Date: 2020-07-14
山东迈特新材料科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But it has the following problems: 1) The molecular weight is small and the water solubility is very large, so the compatibility with the polymer is not good, and it is easy to migrate, and the water resistance of the flame-retardant products made is poor; 2) The thermal stability is poor [Wei Lifei, Zhu Zhiguo , Jin Xinyi, et al. Effects of intumescent flame retardants based on tris(2-hydroxyethylisocyanurate) on the combustion properties of polymers. Journal of Textile Science, 2017, 38(9): 24-30; Li Yongqiang. Insoluble Dispersion polymerization of ammonium polyphosphate and its flame retardant effect on polypropylene. Master's degree thesis of Qingdao University of Science and Technology, 2012-06)
The above two kinds of polyester derivatives of Saike have successfully solved the problems of small molecular weight, high water solubility, poor compatibility with polymers and easy migration of Saike, but compared with Saike, the carbon-forming performance has declined. In particular, due to the large molecular weight of terephthalic acid, the proportion of triazine ring in the polyester molecule is small, and the charcoal performance of derivatives of terephthalic acid polyester is greatly reduced, and the derivatives of maleic anhydride Because it contains a large number of double bonds, its thermal stability is poor, and it is easy to turn yellow when heated, which limits its use

Method used

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  • THEIC derivative and preparation method thereof
  • THEIC derivative and preparation method thereof

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preparation example Construction

[0021] Preparation of flame-retardant PP samples: PP and IFR are mixed in a JS30A twin-screw extruder (Yantai Qitong Powder Machinery Co., Ltd.) at 190-200°C with a twin-screw speed of 20-30rpm at a mass ratio of 72:28. Extrude, mix and granulate under certain conditions. The dried granules are molded with a 2G-10T precision automatic tablet press (Dongguan Zhenggong Electromechanical Equipment Technology Co., Ltd.) at 200-210°C under a pressure of 5MPa, then cold-pressed under a pressure of 5MPa, and then cut into the desired size. Specification of splines is required for performance testing.

[0022] 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×3.2mm.

[0023] The polypropylene (PP for short) used in the present invention is the PPT30S type polypropylene produced by Yan'an Energy Ch...

Embodiment 1

[0025] Add 500.4g (5mol) of succinic anhydride, 1049g (4mol) of Sike and 49g of sulfuric acid into a 5L kneader equipped with a reflux condenser, water separator, stirrer and thermometer, and heat up to 160±5°C for 6 hours. Then cool down to room temperature, pulverize to -200 mesh with a universal pulverizer, wash with 500mL deionized water, repeat the washing 3 times, and dry the washed filter cake at 110°C to constant weight to obtain 1430g white powder product. The solubility of the product is 0.19g / 100mL water. Thermogravimetric analysis shows that the thermal stability of product is good, and the temperature (referred to as T respectively) when losing weight 2%, 5% and 10% 2wt％ , T 5wt％ and T 10wt％ ) and the temperature at the maximum thermogravimetric rate (T max ) are 274.3°C, 305.2°C, 372.5°C and 404.9°C, respectively.

[0026]attached figure 1 Medium, 3446.60cm -1 It is the O-H intermolecular hydrogen bond stretching vibration peak, 2972.20cm -1 for -CH 2 The...

Embodiment 2

[0029] Add 500.4g (5mol) of succinic anhydride, 1049g (4mol) of Sike and 49g of sulfuric acid into a 5L kneader equipped with a reflux condenser, water separator, stirrer and thermometer, and heat up to 180±5°C for 4 hours. Then cool down to room temperature, pulverize to -200 mesh with a universal pulverizer, wash with 500mL deionized water, repeat the washing 3 times, and dry the washed filter cake at 110°C to constant weight to obtain 1428g white powder product. The solubility of the product is 0.20g / 100mL water. Thermogravimetric analysis showed that the thermal stability of the product was good, T 2wt％ , T 5wt％ , T 10 and T max They are 273.1°C, 297.7°C, 351.9°C and 401.5°C, respectively.

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Abstract

The invention discloses a THEIC derivative. The derivative is prepared by polycondensation by taking THEIC and succinic acid compounds (succinic acid and butanedioic anhydride) as raw materials and taking strong protonic acid as a catalyst. The method comprises the following specific steps: adding THEIC, the succinic acid compound and the catalyst into a kneading machine provided with a reflux condenser, a stirrer and a thermometer, heating to 120-200 DEG C, carrying out heat preservation reaction for 2-8 hours, cooling to room temperature, grinding to 200 meshes, washing with deionized waterfor three times, and drying the washed filter cake at 110 DEG C to constant weight to obtain a white powdery product. The derivative has the advantages that bulk polymerization is adopted, the preparation process is simple, basically no three wastes are discharged, and the derivative not only has good char forming property and thermal stability, but also has low water solubility, good compatibility with polymers, cheap raw materials and wide sources. The THEIC derivative can be used as a charring agent of an intumescent flame retardant.

Description

technical field [0001] The present invention relates to a kind of three (2-hydroxyethyl) isocyanurate (abbreviated THEIC or Sai Ke) polyester derivatives and preparation method thereof, specifically with Sai Ke and succinic acid compounds as The raw material is a syke polyester derivative prepared by polycondensation, and the compound can be used as a char-forming agent of an intumescent flame retardant, and belongs to the field of chemical 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, With the advantages of low smoke, low toxicity, and less addition, it meets the requirements of current flame retardant materials for smoke suppression and low toxicity, and is considered to be a green flame retardant with great development potential...

Claims

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Application Information

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IPC IPC(8): C08G63/685C08G63/78C08L23/12C08L67/00C08K3/32
CPCC08G63/6854C08G63/78C08L23/12C08L2201/02C08K2003/323C08L67/00C08K3/32
Inventor 郭建树刘俊宏杨喜生赵震唐林生
Owner 山东迈特新材料科技有限公司
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