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Triazine compound coordination crosslinking synergistic agent for elastomer and preparation method thereof

A technology of coordination crosslinking and triazines, which is applied in the field of preparation of hydroxyalkane chain-substituted triazines, can solve problems such as unreported research, and achieve improved crosslinking efficiency, strong chemical reactivity, and good coordination crosslinking. synergistic effect

Inactive Publication Date: 2011-09-14
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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  • Triazine compound coordination crosslinking synergistic agent for elastomer and preparation method thereof
  • Triazine compound coordination crosslinking synergistic agent for elastomer and preparation method thereof
  • Triazine compound coordination crosslinking synergistic agent for elastomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 15mL of acetone to a 200mL four-neck flask equipped with a reflux device, a stirrer, a constant pressure dropping funnel and a thermometer, place the flask in an ice-salt bath, and control the temperature at 1°C to 3°C, then add 1.8450g (0 .010mol) cyanuric chloride, stir and disperse evenly, join 1.0514g (0.010mol) diethanolamine in the cyanuric chloride solution, stir, meanwhile, a small amount of sodium hydroxide solution (0.40gNaOH is dissolved in 10mL distilled water ), control the pH value of the reaction system between 7.0±0.2, and react for 3 hours to obtain the intermediate product Ia 1 . Intermediate Ia 1 It is 2-(N,N-dihydroxyethyl)amino-4,6-dichloro-1,3,5-triazine compound, the theoretical structural formula is as follows:

[0030]

[0031] Intermediate Ia 1 Does not require separation and purification, to contain Ia 1 Add 15mL of water to the reaction solution, accelerate stirring evenly, then put 2.2079g (0.021mol) diethanolamine into the soluti...

Embodiment 2

[0037] Add 15 mL of N,N-dimethylacetamide-acetone mixed solvent with a volume ratio of 1:1 to a 200 mL four-neck flask equipped with a reflux device, a stirrer, a constant pressure dropping funnel and a thermometer, and place the flask on ice In the brine bath, the temperature is controlled at -1°C ~ 1°C, then add 1.8450g (0.010mol) cyanuric chloride, stir and disperse evenly, add 1.4651g (0.011mol) diisopropanolamine to the cyanuric chloride solution, stirring, and at the same time, a small amount of potassium hydroxide solution (0.56gKOH dissolved in 10mL distilled water), control the pH value of the reaction system between 6.5±0.2, and react for 1.5 hours to obtain the intermediate product Ia 2 . Intermediate Ia 2 It is 2-[N,N-di(2-hydroxy)propyl]amino-4,6-dichloro-1,3,5-triazine compound, the theoretical structural formula is as follows:

[0038]

[0039]Intermediate Ia 2 Does not require separation and purification, to contain Ia 2 Add 20mL of water to the reaction...

Embodiment 3

[0045] Add 20mL of tetrahydrofuran to a 200mL four-necked flask equipped with a reflux device, a stirrer, a constant pressure dropping funnel and a thermometer, place the flask in an ice-salt water bath, and control the temperature at 0°C to 2°C, then add 1.8450g (0.010 mol) cyanuric chloride, stir and disperse evenly, join 3.1392g (0.011mol) phenyl diisopropanolamine in the cyanuric chloride solution, stir, simultaneously, a small amount of sodium carbonate solution (0.53gNa 2 CO 3 dissolved in 10mL distilled water), control the pH value of the reaction system between 6.5±0.2, and react for 2 hours to obtain the intermediate product Ia 3 . Intermediate Ia 3 It is 2-[N,N-bis(1-phenyl-2-hydroxy)propyl]amino-4,6-dichloro-1,3,5-triazine compound, the theoretical structural formula is as follows:

[0046]

[0047] Intermediate Ia 3 Does not require separation and purification, to contain Ia 3 Add 25mL of water to the reaction solution, accelerate the stirring evenly, then ...

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Abstract

The invention relates to a method for preparing a triazine compound coordination crosslinking synergistic agent for elastomers, and particularly for preparing a hydroxyalkyl chain substituted triazine compound. The method is characterized in that cyanuric chloride and dihydric alcohol are used as raw materials; the cyanuric chloride and the dihydric alcohol are allowed to react by a nucleophilic substitution reaction in an organic solvent medium; a few amount of a lewis base aqueous solution is added dropwisely to control the pH of the system; after the lewis base aqueous solution is added completely, an intermediate Ia is obtained; water is added into an Ia-containing reaction solution as a solvent; dihydric alcohol with a molar ratio to the intermediate of 2-2.2 is added at room temperature; the temperature is increased controllably; by-product hydrogen chloride is absorbed by the lewis base aqueous solution; the pH of the reaction system is controlled; and the triazine compound as the target product is obtained. The hydroxyalkyl chain substituted triazine compound obtained by the method of the invention comprises six hydroxyls and six nitrogen atoms, has strong chemical reactivity, is easy to participate in a coordination crosslinking reaction, and can be used as a crosslinking synergistic agent in an elastomer curing system.

Description

technical field [0001] The invention relates to a method for preparing a triazine compound coordination cross-linking synergist for elastomers, in particular for the preparation of hydroxyalkane chain-substituted triazine compounds, which are mainly used as coordination cross-linking synergists for elastomers, Flame retardant synergist for elastomers, initiator for synthesis of pharmaceuticals, dendrimers and hyperbranched polymers. Background technique [0002] Since the discovery of thermoplastic elastomers (TPE) in the 1940s, four classes of thermoplastic elastomers have been developed, which are different from traditional covalently cross-linked thermosetting elastomers: they are all realized by non-covalent bonds Cross-linking includes hydrogen bond cross-linking, van der Waals force cross-linking, ionic cross-linking and coordination cross-linking. Thermoplastic elastomers can realize continuous and rapid processing technology and direct recycling of leftovers and was...

Claims

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Application Information

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IPC IPC(8): C08K5/3492C07D251/70C08G83/00
Inventor 肖荔人姜明陈庆华陈荣国钱庆荣
Owner FUJIAN NORMAL UNIV
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