The method of obtaining fire protective chemical fibers

 

(57) Abstract:

Usage: the technology for production of fire-protected fibers. The inventive chemical fibers treated in the aquatic environment of the redox system consisting of salts of ferrous iron and hydrogen peroxide, and grafted on fiber 2-(0-isobutylacetophenone)-methylpropenoate when the concentration in the reaction medium 5 - 7 wt.%. Oxygen index before/after 10 washings, %: viscose fiber 29,5 to 30.1/29,3 - 29,9, polyester fiber 30,3/30,0, polycaproamide fiber 28,7/28,4. table 1.

The invention relates to a technology for fire protective chemical fibers, particularly synthetic (rayon) and synthetic (nylon, polyester). Fire protective chemical fiber intended for the manufacture of decorative fabrics used in institutions with mass stay of people (hospitals, hotels, railway transport, and so on), as well as for the manufacture of clothing for various purposes.

A method of obtaining fire protective polyamide (PA) fibers by grafting to PA polyacrolein with subsequent processing dimethylphosphite or antimony chloride /1, 2/. Adnah">

A method of obtaining fire-protected graft copolymers of cellulose with the use of phosphorus-containing monomers, for example-phenylphosphinic acid by pretreatment with aromatic amines in the molecule of the cellulose, followed by converting them into diazogroup with the aim of initiating graft polymerization /3/. The disadvantage of this method is a multistage process.

Closest to the invention is a method for fire-protected fibers of regenerated cellulose by grafting after processing in the aquatic environment of the redox system Fe+2- H2O2poly-2-methyl-5-vinylpyridine) - derivatives (PMVP), followed by processing of a copolymer of cellulose with PMIT 1,0 2,0% aqueous solution of polyphosphoric acid at 20 60oC for 10 to 20 minutes, rinsing, wringing and drying /4, 5/.

The main disadvantages of this method are

the two-phase process process

reducing fire retardant properties after repeated water treatments,

low efficiency of the flame retardant action of phosphoric acid salt PMIT for synthetic fibers.

The technical object of the present invention is increased the s and the reduction process.

This task is solved by a method of obtaining fire-protected fibers by processing in the aquatic environment of the redox system Fe+2H2O2and a grafting monomer, and according to the invention as a monomer using 2-(0-isobutylacetophenone)methylpropenoate with a concentration of 5 to 7 wt. in the reaction medium.

2-(0-isobutylacetophenone)methylpropenoate (BMTN) are obtained in a known manner /6/. Vaccination is carried out by a known method using as the initiator of the well-known redox systems consisting of salts of ferrous iron and hydrogen peroxide, in known conditions /5/.

At lower concentrations of phosphorus-containing monomer is less than 5 wt. modified fibers do not have flame-retardant properties (oxygen index KI < 27%). When the concentration of BMTN above 7 wt. dramatically increases the number of grafted homopolymer, reduced the number of grafted polymer and worse physical and mechanical properties of modified fibers.

The method can be implemented at known operating equipment.

The test results of the samples listed in the table.

Pria (salt Mora) at a pH of 4.4 to 5.0 and 20oC for 20 min. Press. Then the fiber is placed in a 5% aqueous solution BMTN. In the reaction mixture is heated to 40oC, add 0.03 wt. H2O2and after heating up to 80oC conduct a vaccination for 90 min, after which the sample is washed with hot water (80 to 90oC) for 20 minutes, wring out and dry.

Example 2. 100 g of viscose fibers pre-treated with 0.25% aqueous solution of salt Mora at pH 4.5 to 5.0, and 20oC for 20 min. Press. Then the fiber is placed in a 7% aqueous solution BMTN. In the reaction mixture is heated to 40oC, add 0.03 wt. H2O2and, after heating to 90oC conduct a vaccination for 90 min, after which the sample is washed with hot water (80 to 90oC) for 20 minutes, wring out and dry.

Example 3. 100 g of polyester fiber polyester pre-treated with 0.25% aqueous solution of salt Mora for 20 min at a temperature of 20oC. Press. The sample was then placed in a 6% aqueous solution BMTN. The reaction mixture is heated to 40oC, add 0.03 wt. H2O2and, after heating to 90oC conduct a vaccination for 90 min, after which the fiber is washed with hot water (80 to 90oC) for 20 minutes, wring out Il salt Mora at pH 4.5 to 5.0, and 20oC for 20 min. Press. Then the fiber is placed in a 7% aqueous solution BMTN. In the reaction mixture is heated to 40oC, add 0.03 wt. H2O2and, after heating to 90oC conduct a vaccination for 90 min, after which the fiber is washed with hot water (80 to 90oC) for 20 minutes, wring out and dry.

Example 5 (prototype). 100 g of viscose fibers pre-treated with an aqueous 0.25% salt solution Mora at pH 4.5 to 5.0, and 20oC for 20 min. Press. Then the fiber is placed in a 3% aqueous solution of acetic acid salt of 2-methyl-5-vinylpyridine) - derivatives. In the reaction mixture is heated to 40oC add to 0.025 wt. H2O2and, after heating to 80oC carry out the reaction for 120 min, after which the sample is washed with 0.5% solution of acetic acid, then with water and dried.

The obtained graft copolymer of cellulose containing about 13% poly-2-methyl-5-vinylpyridine) - derivatives (PMVP), is treated at a temperature of 2 25oC a 2.0% aqueous solution of polyphosphoric acid for 45 min, washed with distilled water until neutral wash water and dried.

Example 6 (prototype). 100 g of the fibers of the graft copolymer polyester with PMIT obtained as opisannyi PMIT 13 wt.), process at room temperature of 2.0% aqueous solution of polyphosphoric acid for 45 min, washed with distilled water until neutral wash water and dried.

Example 7 (prototype). 100 g of the fibers of the graft copolymer of polycaproamide with PPSP, obtained as described in example 5, using the redox of Fe+2H2O2(contents PMIT 14%) treated at room temperature of 2.0% aqueous solution of polyphosphoric acid for 45 min and washed with distilled water until neutral wash water, and dried.

As can be seen from table, the invention allows to significantly improve the stability of the flame retardant effect to wet treatments (decrease KEY after 10 washings, does not exceed 0.2 to 0.3 units) and flame retardant characteristics of chemical fibers. Using phosphorus-containing monomer BMTN were obtained fire protective PE and PA materials with KI, is 28.7 and 30.3%, respectively. At the same time using a known method on the prototype to get a fire-protected PA and PE fiber is not possible (CI 25,0 27,1%).

The method of obtaining fire protective chemical fiber>and a grafting monomer, characterized in that, as a monomer using 2-(O-isobutyl, methylphosphonate)methylpropenoate with a concentration of 5 to 7 wt. in the reaction medium.

 

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