SU1671668A1 - Cross-linked phosphorus-containing polyether acrylate as fike-resistant film material and process for preparing thereof - Google Patents

Abstract

This invention relates to the chemistry of polymers and can be used to create slow-burning materials. The invention makes it possible to create organophosphorus polyether acrylates possessing the properties of flame retardant film materials with an oxygen index of 20–32%. Polyether acrylate of the general formula @ where X = 0.19 - 0.32 ppm, Y = 0.68 - 0.81 ppm when R = (CH ₂ CH ₂ O) ₃

X = 0.31 - 0.46 ppm, Y = 0.54 - 0.69 ppm when R = (CH ₂ CH ₂ O) ₃ -C-OC-O (CH ₂ CH ₂ O) ₃ , is obtained by copolymerization of a mixture of 20-30% by weight of 3,4-dichloro-1,3-butadiene-2 dimethyl ether phosphonic acid with 70–80 wt.% TGM-3 or MHD-9 under the action of a catalytic system consisting of cumene hydroperoxide, cobalt linoleate and manganese trisacetylacetonate when heated in a thin layer on a glass substrate. 2 sec. f-ly, 2 tab.

Description

The invention relates to the chemistry of polymers, in particular to phosphorus-containing polyether acrylates and the process for their preparation, and can be used in technology to create fire-resistant film materials with increased fire safety requirements.

The aim of the invention is the creation of phosphorus-containing polyether acrylates as a fire-resistant film material.

Dimethacrylate-bis-triethylene-ethanol phthalate (MGF-9) is used as the initial oligoether acrylates, where

, triethylene glycol dimethacrylate (TSH-3), where R - (OCHNSNg -) - 3. MGF-9 is a colorless non-volatile viscosity liquid (100-150) at HU 6m2 / s or 100-150 cSt with a degree of polymerization equal to one; ,20

mol.m. 540, d

1.165,

1.4891, MGF-9 is dissolved in alcohol, chloroform, acetone, ether, tetrahydrofuran, benzene, and other organic solvents. TGM-3 is a colorless transparent liquid Ј in ecost (10-30). 1 (G6m2 / s or 10-30 cSt with a degree of polymerization of one: mol.m. 281, d 1.0922, n 1.4621. TS-3 is dissolved in alcohol, acetone, chloroform, ether, chlorobenzene, tetrahydrofuran and others. Solvents. Dimethyl 3,4-dichloro-1, 3-butadiene-2-phosphonic acid (DMHBP) is synthesized from dichloro-anhydride-3,4-dichloro-1,3-butadiene-2-phosphonic acid and methyl alcohol.

This monomer is

- colorless liquid with T

kip

75 ° C /

/ 0.5 gf, 1.5050, d - 1.3681 Example (control, outrageous values of type n.). 0.045 g (3 wt.%) Of cumene hydroperoxide, 0.341 g (0.5 wt.%) Of cobalt linoleate are added to a mixture of 1.35 g of TSP-3 and 0.15 g of DMKHBP (10% by weight of the initial monomer mixture). and 0.0015 g (0.1 wt.%) manganese tris-acetylacetonate (TAM), the mixture is stirred until a homogeneous mass is obtained and poured onto glass plates, which are placed in a thermostat, where they are copolymerized for 240 minutes at 110 ° WITH. Yield of a spatially networked copolymer. (after extraction in chloroform for 6 hours) is 1.44 g (96%). The values of x and y - - ЈR - - (CHgCHjO jl, and the properties of the polyether acrylate are given in Table 1 and

Example2. R mixture of 1.2 g TS-3 and 0.3 g DMHBP (20% by weight of the starting monomer mixture) was added 0.045 g (3% by weight) of cumene hydroperoxide, 0.341 g (0.5% by weight) of cobalt linoleate and 0.0015 g (0.1 wt.%) TAM. Further, all operations are performed as in example 1. The output of the copolymer (selected

The spatially reticulated copolymer is carried out analogously to the example) 1.38 g (92%)

The values of and for and the properties of the polymer are given in Tables 1-3. The data in examples 3-26 are given in table 1-3.

The degradation products of phosphorus-containing polyether acrylates released by combustion have a MAC of 5 mg / m3 versus the known 2.5 mg / m3.

Claims (2)

1. Phosphorus crosslinked polyether acrylate of general formula -H2C-C CC1-CHC1 H, CO-P-OCH3 I 3 o CH-CH, I h (h -) - H2C-C-C-CH  . shu 0-r-0 where x X 0.19-0.32 ppm, y - 0.68- 0.81 ppm with R - (- CH2CH20) 3; 0.31-0.46 ppm, y - 0.54-0.69 ppm. with R - (), f-0- (CH7CH20) f, about as a flame retardant film material. 2. A process for the preparation of a phosphorus-containing crosslinked polyester acrylate of the general formula -f- NgC-OCC1-CHC) 3- H3CO-P-OCVI3 O 9nz ™ 3 --H-C-C-C-CH, z I I z oo I I 0-r-0 x 0.19-0.32 ppm, y 0.68 0, 81 ppm when R - (-CH2CH20) 5; x - 0.31-0.46 ppm, y - 0.54 - 5 0.69 ppm when R - (-SNgNGO) 35 -0- (CH2CH20} 35 The mixture consisting of 0.75-1.35 mash onto the glass n-5 substrate. 3,4-dichloro-1,3-butadiene-2-phosphonic acid dimethyl ester with 0.75-0.155 mash. dimethacrylate triethylene glycol or dimethacrylate of bis-tri-ethylene glycol phthalate with an initiating system consisting of 2.5-3.5% by weight of cumene hydroperoxide, 0.40-0.50 Mac.Z cobalt linoleate and 0.1-1.0 wt.1 tris-acetylacetonate manganese in the calculation of the mixture of comonomers, and the subsequent heating of the mixture at 1100 115 ° C for 120-240 minutes Spreadsheets The conditions of the process of sopoinherniacine oligoether acrylates with 3,4-dichloro- |, e-vutadien-2-phosphono-dimethyl dimethyl ether 1kTGM-E90,010,0 Linomat cobalt Cumene hydroperoxide 0, wt.2 TAI Bis- (methacryloyloxyethylenecarbonate) -2,2-dinetylpropavd ol-1,3-Ois- (D-chloroethyl) - 6-vron and the phosphonate is used.  Bis- (triethylglycol) phalate-nv- (i-chloro-tnl) -1s-bromo-vin-phosphonate dnmetacrylate is used. 240 BUT 96 Other according to the co-imeriation of TP1-E with DIHPF p topkom layer on the air according to example 2 Table 2