Phosphorus-boron-containing methacrylate as polyvinyl alcohol-base film material combustion inhibitor

FIELD: chemistry of organophosphorus compounds.

SUBSTANCE: invention relates to compounds with the bond C-P, namely to phosphorus-boron-containing methacrylate that can be used as inhibitor of combustion of polyvinyl alcohol-base film materials. Invention describes phosphorus-boron-containing methacrylate of the following formula: wherein n = 4-8. Polyvinyl alcohol films modified with indicated phosphorus-boron-containing methacrylate shows the enhanced refractoriness, rupture strength up to 206 kgf/cm2, water absorption up to 240% and relative elongation up to 12%.

EFFECT: valuable properties of substance.

1 tbl, 2 ex


The invention relates to the field of chemistry of organophosphorus compounds with C-P bond, namely phosphoriboisomerase the methacrylate, which can be used as a fire retardant film materials based on polyvinyl alcohol.

Know the use of β-methacryloxypropyltrimethoxysilane as modifiers to make the polymers of increased fire resistance (USSR Author's certificate No. 528303, CL 07 F 9/40. Publ. 15.09.76).

Known application α-methacryloyloxyethyl as monomers for obtaining a flame-retardant polymers (USSR Author's certificate No. 584009, CL 07 F 9/40. Publ. 15.12.77).

However, the relatively low phosphorus content in the data structure modifiers are not to be used in low concentrations, which in turn leads to deterioration of operating properties.

The closest structure and neschastiu is a phosphorus-containing olygoesteracrylate (USSR Author's certificate No. 598909, CL 07 F 9/40. Publ. 25.03.78).

However, along with a low phosphorus content this modifier is insoluble in water, which does not allow to combine it with aqueous solutions of polyvinyl alcohol (PVA).

Object of the present invention to provide a new effective inhibitor of combustion, the which is well combined with the aqueous solutions of polyvinyl alcohol and provides film materials based on it, having a high resistance.

The technical result of using the proposed inhibitor of combustion is receiving film materials based on polyvinyl alcohol, which is characterized by high resistance, tensile strength and elasticity.

The technical result is achieved by the fact that as a fire inhibitor use a new connection - phosphoriboisomerase methacrylate of the formula:

where n=4-8.

We offer new phosphoriboisomerase methacrylate (BMF) is produced by interaction phosphoriboisomerase oligomer and glycidylmethacrylate.

The presence in the structure of atoms of phosphorus and boron, which are inhibitors of combustion, increases technical and economic effect from the use of this modifier. In addition, high concentrations of phosphorus in the structure of the substance contributes to the achievement of the maximum result without resorting to the use of large concentrations. In addition, good compatibility with aqueous solutions of polyvinyl alcohol, which can be explained by the possible formation poluvsasavania mesh and features of the interfacial interaction of the linear thermoplastic polymer (PVA), and spatial cross-linked polymer formed by polymerization of polyfunctional oligomer (BMF), which allows to make a conclusion about the actual application phosphoriboisomerase methacrylate for the modification of polyvinyl alcohol.

Synthesis phosphoriboisomerase methacrylate was carried interaction phosphoriboisomerase oligomer with glycidylmethacrylate in accordance with reaction scheme:

Interaction phosphoriboisomerase oligomer and glycidylmethacrylate conducted in the medium of dimethylformamide (acetone, water). The reaction proceeds with evolution of heat and formation of a viscous transparent solution BMF.

The invention is illustrated by the following example.

Example 1. In chetyrehosnuju flask equipped with stirrer, reflux condenser, thermometer and drip funnel, load 5 g of borate methylphosphate, 82.6 ml of acetone and stirred at 22-23°until dissolved. Download 0.03 g of hydroquinone. With stirring from a dropping funnel is added 6.59 g glycidylmethacrylate with such speed that the temperature of the reaction mixture did not exceed 30°C. After the addition of glycidylmethacrylate the reaction mass is stirred for 5 hours. The mixture is then heated to 60°C for 5 hours. The liquid fraction is extracted with acetone, United remains is filtered off, the solvent is removed in vacuum. The crystalline residue is filtered off, the solvent is removed in vacuum. Output connections 4.1 g (35.2%). The reaction product is a very viscous liquid amber in color, soluble in water, is cetone, toluene, alcohols; nD20=1.4612, d420=1/7069 g/cm3v=31.2. Article IR spectrum (liquid paraffin), v, cm-1: 3396, 2880, 2430, 1748, 1640, 1456, 1336, 1156, 1060. Range PMR(GMFM-d),δ, ppm:1,13, 1,34-1,48, 1,96, 2,18, 37, 4,19, 5,25, 5,71, 6,1, 8,48, 9,07 an NMR Spectrum31P (GMFM-d),δppm:3,83.6,54,28 .16. Found, %: From 34.5, N 4,24, P 12,29. Calculated, %: From 33.7, N. Android 4.04, P 12,4, Mg=960-1920.

Example 2. The modification was carried out by mixing aqueous solutions of PVA and BMF in different ratios, followed by the application of polymer solutions onto a glass surface and exposure at room temperature to form films. Then we study the properties of polyvinyl alcohol as Flammability, tensile strength, elongation and water absorption. The study vodopoglascheniya was conducted in accordance with GOST 4650-65, strength characteristics with GOST 20403-75, and the study of the Flammability of the samples in accordance with the procedure under which Flammability of the samples was evaluated by time-extinguishing after exposure to open flames GOST 21793-76. Research results and properties of the unmodified polyvinyl alcohol shown in the table.


Properties of thin film materials
Properties Unmodified PVAThe concentration of the BMF,%
The tensile strength, kgf/cm295206.3188.2
Water absorption, %20.5235.2240.1

As can be seen from the presented data, phosphoriboisomerase methacrylate is an effective fire retardant film materials based on polyvinyl alcohol. When using BMF different concentrations of speed-extinguishing reduced. Add in the weight of BMF from 1.0 to 15.0% does not samozatuhaniya, i.e. film burn completely, and adding 16% PWM film Samosata. Research strength at break of the samples showed that when using 8% BMF strength is increased compared to the unmodified sample (95 kgf/cm2) to 206.3 kgf/cm2and then begins to fall. Thus there is an inverse dependence of the relative elongation of the concentration SEM. This suggests that the modified film become more elastic. Videopost the e was estimated by the change of the mass of the sample after soaking it in water overnight at room temperature. Then the observed increase in mass of the samples with increase in the content of BMF almost more than 10 times. Hence, leaching BMF does not occur. The concentration increase of over 16% leads to deterioration of strength at break, and the rest of the monitored properties virtually unchanged.

Thus, the above data confirm that the implementation of the use of the claimed invention the following cumulative conditions:

the tool embodying the claimed invention when it is used, intended for use as fire retardant film materials based on polyvinyl alcohol;

for the claimed invention in the form as it is characterized in the claims, confirmed the possibility of its implementation using the steps described in the application and known before the priority date tools and methods;

the tool embodying the claimed invention in its implementation, is able to achieve a technical result.

Therefore, the claimed invention meets the requirement of "industrial applicability".

Phosphoriboisomerase methacrylate of the formula

as fire retardant film materials based on polyvinyl alcohol.


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