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A kind of hyperbranched polysiloxane and preparation method thereof

A technology of polysiloxane and propyltriethoxysilane, applied in the field of hyperbranched polysiloxane and its preparation, can solve the problems of harsh conditions, high self-polymerization temperature of alkynyl groups, use of flame retardants, etc. Excellent heat resistance and rigidity, good processability, easy reaction temperature effect

Active Publication Date: 2020-07-21
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the polymerization temperature of alkynyl compounds is relatively high (≥320°C), which cannot match the curing process of existing heat-resistant thermosetting resins
[0007] Chinese invention patent (CN104327269A) discloses a hyperbranched polysiloxane containing a macrocyclic structure and its synthesis method. Alkyne groups are grafted on the hyperbranched polysiloxane, but there are four problems as follows: First, the alkyne The self-polymerization temperature of the base is high
Second, the preparation process is complicated and the conditions are relatively harsh
Halogen-containing flame retardants have become banned substances in many international laws and regulations. In other words, the hyperbranched polysiloxane containing alkyne groups cannot be used as flame retardants.
Fourth, the synthetic product is solid, which makes hyperbranched polysiloxane lose the advantage of low viscosity

Method used

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  • A kind of hyperbranched polysiloxane and preparation method thereof
  • A kind of hyperbranched polysiloxane and preparation method thereof
  • A kind of hyperbranched polysiloxane and preparation method thereof

Examples

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Embodiment 1

[0038] See attached figure 1 , which is a schematic diagram of the synthesis principle of hyperbranched polysiloxane provided in this example; the synthesis of hyperbranched polysiloxane mainly includes two steps: the first step is isocyanate propyltriethoxysilane and 3-amino Phenylacetylene reaction; the second step is the generation of hyperbranched structure. Concrete process conditions and steps are as follows:

[0039] 1. Add 0.1mol of 3-aminophenylacetylene and 0.1mol of isocyanate propyltriethoxysilane into a flask containing 20mol of toluene; react at 60°C for 12h under nitrogen protection and magnetic stirring; spin Intermediate A was obtained after removal of the solvent by evaporation.

[0040] 2. Dissolve intermediate A in 20 mol of ethanol and put it in a flask, then add 0.102 mol of water into the flask, react at 60°C for 6 hours; then evaporate the solvent at 40°C, wash the product several times with ethanol, Product B is obtained. Product B was vacuum-dried...

Embodiment 2

[0066] Add 0.1mol of 3-aminophenylacetylene and 0.1mol of isocyanatopropyltriethoxysilane into a flask containing 10mol of carbon tetrachloride, and react at 100°C for 24h under nitrogen protection and magnetic stirring; Intermediate A was obtained after pressure distillation to remove the solvent. Dissolve intermediate A in 10 mol of methanol, then add 0.12 mol of water into the flask, react at 80°C for 12h; then remove the solvent at 40°C, wash the product several times with methanol to obtain product B. The product B was vacuum-dried at 80° C. for 12 hours to obtain a yellow liquid, which was hyperbranched polysiloxane.

Embodiment 3

[0068] Add 0.1 mol of 3-aminophenylacetylene and 0.1 mol of isocyanatopropyltriethoxysilane to a flask containing 40 mol of chloroform, and react at 60°C for 8 hours under argon protection and magnetic stirring; rotary evaporation method After removal of the solvent, intermediate A is obtained. Intermediate A was dissolved in 40 mol of propanol, then 0.2 mol of water was added to the flask, and reacted at 40°C for 4 hours; then the solvent was evaporated at 40°C, and the product was washed several times with propanol to obtain product B. The product B was vacuum-dried at 40° C. for 4 hours to obtain a yellow liquid, which was hyperbranched polysiloxane.

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Abstract

The invention discloses hyperbranched polysiloxane and a preparation method thereof. The preparation method comprises the following steps of enabling aminophenylacetylene and a silane coupling agent to react, so as to obtain alkynylated silane; then reacting with water, so as to form the hyperbranched polysiloxane. The prepared hyperbranched polysiloxane has the characteristics that the elements harmful to a human body are not contained, the hyperbranched polysiloxane is in a liquid state at normal temperature, and contains a large amount of hydroxyls or secondary amine groups and other activegroups, and the good material guarantee is provided for the modifying of polymer and the research and development of new materials; because the self-polymerizing temperature of alkynyl is not higherthan 200 DEG C, the polymerizing at the curing temperature of resin is realized; the good heat-resistant property and rigidity of the modified resin are realized by the hyperbranched polysiloxane. A synthesizing method of the hyperbranched polysiloxane containing the alkynyl has the characteristics that the technology is simple, the scaled production is easily realized, and the like.

Description

technical field [0001] The invention relates to a halogen-free and phosphorus-free flame retardant and a preparation method thereof, in particular to a hyperbranched polysiloxane and a preparation method thereof. Background technique [0002] Flame-retardant polymer materials have become urgently needed functional polymer materials in many fields. An effective way to prepare flame-retardant polymer materials is to add flame retardants. [0003] Phosphorous flame retardants (PFRs) are currently the most widely used types of halogen-free flame retardants. However, PFRs have poor heat resistance, and when added to heat-resistant thermosetting resins, the initial thermal decomposition temperature (Tdi) of the resin is often lowered. In addition, recent studies have shown that PFRs have bioaccumulation, which affects the ecological environment and human health. Therefore, it is a meaningful work to develop halogen-free and phosphorus-free flame retardants suitable for heat-resi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/26C08G77/06
Inventor 顾嫒娟张志娟梁国正袁莉
Owner SUZHOU UNIV
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