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Chemical magnesium hydroxide particle surface modification method for flame resistance of leather

A magnesium hydroxide and particle surface technology, which is applied in the treatment of dyed polymer organic compounds, fibrous fillers, textiles and papermaking, etc., can solve problems such as no public reports, and achieve a firm combination

Active Publication Date: 2012-07-25
CHINA LEATHER & FOOTWEAR IND RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, atom transfer radical polymerization (ATRP) has only been developed in recent years. It has attracted much attention for its mild reaction conditions, wide range of applicable monomers and controllable polymerization process. It has been successfully applied to inorganic silica, cellulose, nuclear polymerization Surface modification of sugar particles, starch particles, polypeptides, etc. However, there is no public report on the surface modification of magnesium hydroxide particle surface through atom transfer radical polymerization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 5.0g magnesium hydroxide, 100ml toluene, and 10ml 3-aminopropyltriethoxysilane (KH550) into a 250ml three-necked flask, stir magnetically in an oil bath at 110°C, and reflux for 24 hours. The product was washed with excess toluene and acetone and dried in vacuum at room temperature for 24 hours to obtain coupling agent pretreated magnesium hydroxide particles Mg(OH) 2 -NH 2 . Add 50ml dichloromethane and 2.0g Mg(OH) to a 100ml round bottom flask 2 -NH 2 , 6.0ml anhydrous pyridine, 6.0ml initiator 2-bromoisobutyryl bromide, stir at room temperature for 24 hours to obtain the macroinitiator Mg(OH) 2 -Br, X-ray photoelectron spectroscopy (XPS) analysis shows that the percentage of Br on the surface of magnesium hydroxide particles is 0.48%.

[0024] 0.20g macroinitiator Mg(OH) was added to a 100ml single-necked flask 2 -g-Br, 5.0ml glycidyl methacrylate (GMA) and 10ml dimethylformamide (DMF), bubbling with high-purity nitrogen into the flask for 30 minutes, add 0.043g CuBr...

Embodiment 2

[0026] Macro initiator Mg(OH) 2 -g-Br was prepared as in Example 1. 1.5g of macroinitiator Mg(OH) was added to a 100ml single-necked flask 2 -Br, 5.0ml monomer 2-hydroxyethyl methacrylate (HEMA), 10ml methanol, bubbling with high-purity nitrogen into the flask for 30min, add 0.06g CuBr, 83.0μLPMDETA and 8.3μL 2-bromoisopropylate under nitrogen protection Ethyl butyrate, magnetic stirring, polymerization temperature of 50 ℃, reaction for 5 hours, the product Mg (OH) 2 -g-PHEMA composite particles, the polymer grafting rate is 8.44%. Then for Mg(OH) 2 -g-PHEMA composite particles graft the initiator again to obtain the macroinitiator Mg(OH) 2 -g-PHEMA-Br. X-ray photoelectron spectroscopy (XPS) analysis showed that the Br atom percentage on the surface of the magnesium hydroxide particles was 1.75%.

[0027] Add 0.20g macroinitiator Mg(OH) to a 100ml single-neck flask 2 -g-PHEMA Br, 5.0ml glycidyl methacrylate (GMA) and 10ml dimethylformamide (DMF), bubbling high-purity nitrogen int...

Embodiment 3

[0029] Macro initiator Mg(OH) 2 -g-PHEMA-Br was prepared as in Example 2. 0.20g macroinitiator Mg(OH) was added to a 100ml single-neck flask 2 -g-PHEMA-Br, 5.0ml glycidyl methacrylate (GMA) and 10ml dimethylformamide (DMF), bubbling high-purity nitrogen into the flask for 30 minutes, add 0.043g CuBr, 63μLPMDETA under nitrogen protection, Magnetic stirring, polymerization temperature of 30 ℃, polymerization reaction for 1 hour, the product was washed three times with excess dichloromethane and then vacuum dried at room temperature for 24 hours to obtain Mg(OH) 2 -g-PHEMA-PGMA composite particles. The grafting rate of the polymer was 16.91%, the thickness of the polymer coating layer was 43 nm, the molecular weight of the polymer PGMA was 5721 g / mol, and the molecular weight distribution was 1.46.

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Abstract

The invention relates to a chemical magnesium hydroxide particle surface modification method for flame resistance of leather and in particular relates to a method for introducing polymer brushes to a magnesium hydroxide surface by virtue of an atom transfer radical polymerization (ATRP) method to solve the problem that magnesium hydroxide flame retardants have poor compatibility with leather, arebonded with leather insecurely and are not resistant to washing. To be more exact, the invention provides a method by which the content of polymer brushes introduced to the magnesium hydroxide particle surface can be effectively increased to achieve the aim of obviously improving the chemical magnesium hydroxide particle surface modification effect. Magnesium hydroxide composite particles are prepared by introducing initiators to the magnesium hydroxide particle surface by a two-step method. The polymer brushes introduced to the magnesium hydroxide particle surface are controllable in molecular weight and narrow in molecular weight distribution (MWD). The molecular weight and MWD of the polymers are respectively 5700-14000g / mol and 1.5-1.7. The method has the following beneficial effects:the prepared magnesium hydroxide composite particles and such groups as amino groups and carboxy groups in leather collagen can generate hydrogen bonds quite easily, and stronger interactions exit inthe molecules or among the molecules, so that the magnesium hydroxide particles and the leather can be bonded more securely.

Description

(1) Technical field [0001] The invention relates to a method for chemically modifying the surface of magnesium hydroxide particles for flame retardant leather, in particular to a method for introducing a polymer brush on the surface of a magnesium hydroxide flame retardant through an atom transfer radical polymerization method to solve the problem of magnesium hydroxide flame retardant The compatibility of the agent with leather is poor, the combination is not strong, and it is not washable. (2) Background technology [0002] With the improvement of people's living standards and the continuous enhancement of safety awareness, consumers have put forward higher requirements for the performance of leather products. Leather must not only have a good appearance, natural luster, fine texture, and soft feel, but also must have certain flame retardant properties. Therefore, it is imperative to develop leather with certain flame retardant properties. [0003] At present, research reports ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/28C08F220/32C08F220/34C09C1/02C09C3/10D06M15/21
Inventor 常素芹刘建辉
Owner CHINA LEATHER & FOOTWEAR IND RES INST
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