A method of obtaining a flame retardant composition

 

The invention relates to the production of flame retardant composition for surface treatment and impregnation of combustible cellulosic materials - wood, woven and non-woven materials made of natural and mixed fibers of the paper. The method is a dry mixture of monoammonium phosphate, or deammonification, or mixtures thereof with urea, moistening the mixture, the introduction of 0.5-5.0 wt. % surfactant in the next stage of fusion of the mixture at a temperature of up to 120oTo obtain a product with so pl. 102 to 106oC. Fusion continue to receive product, 20% aqueous solution which has a pH of 5.0 to 6.2. The product is cooled and pulverized with stirring. Improved flame retardant properties. table 1.

The invention relates to the field of surface fire-retardant treatment or impregnation of cellulosic materials such as wood and articles of wood, woven and nonwoven materials made from natural or natural and synthetic fibers, and more specifically to a method for producing flame retardant, suitable for these purposes.

For flame-retardant finishing of textiles textile fibres, especially of linen and cotton, widely used flame retardant agent, presmise of monoammonium phosphate (LFA) and/or DAP and various additives [PCT/GB 89/08137, CL 09 To 21/00, 1989; PCT/GB 90/13699, class D 06 M 11/13, 1990].

As additives, these compositions contain boric acid, sulfate or sulpham ammonium halide or ammonium salt, preferably ammonium chloride. Getting these flame retardants is carried out by dry mixing the components at room temperature, followed by dissolving the mixture in water without heating, or by direct dissolution of the components of the mixture in water without heating. The concentration obtained or working solutions is in the range of 5-40 wt.% on solid matter.

These methods are characterized by the necessity of using large quantities of ballast material is water, which considerably increases the cost of transportation of the product. In addition, these compositions have insufficient flame-retardant properties, and composition [PCT/GB 89/08137] several formulations due to high acidity (pH 5.5) unsuitable for processing tissues due to discoloration of the latter.

In accordance with the patent GB 1171475, 27 3/20, 1969 fire wood get soaking it under pressure in an aqueous solution of DAP or a mixture of DAP and the LFA with the subsequent processing soaked and drained wood in weakly acidic aqueous solution meewasin miniaturist not washed out by precipitation, and fire-treated wood does not decrease with time; in addition, the wood itself becomes hygroscopic.

However, this method has the following disadvantages: the two-phase process; the duration of the process; large loss of working solution for impregnation and high cost because of this impregnated material.

Known flame retardant [WO 96/00763, IPC 6, From 09 To 21/04, 1996] for cellulosic materials (wood, cloth, paper). He is an aqueous solution (1-55 wt.%) a mixture of ammonification (LFA and/or DAP), water-soluble and dissociable ammonium salts, water-soluble salts of metals capable of forming water-insoluble salt with positionname, phosphoric acid, acetic acid and, optionally, functional additives; perhaps the presence of sulfuric or hydrochloric acid; the solution is acidic (pH of 1.5 to 4.3, preferably of 3.5-3.7). The specified composition handle flammable materials impregnated under pressure (wood), dipping or nabrasyvaniem with subsequent drying of the material. Impregnation are in a single phase at normal temperature and pressure up to 16 bar for 2-10 hours; drying is carried out at 60oWith the atmosphere with the gradual lowering of vernona thus the wood contains 15-40 wt.% solids impregnating composition by weight of the tree.

Processing of tissue or paper carried out by dipping or nabrasyvaniem working solution with a concentration of 5-25 wt.%; after wringing the fabric is dried; weight gain of the treated fabric is 10-15 wt.%.

According to the authors treated with the inventive composition materials have a high resistance and weather resistance, low smoke emission.

However, the composition and method for producing fire-retardant materials on WO 96/00763 has the following disadvantages.

1. The working solution has a high acidity (pH of 1.5 to 4.3). It is unlikely that dense wood will be able to neutralize even prolonged drying, because there is addition of acetic acid are present residual phosphate and possibly sulfuric acid, which are difficult to remove. Residual acidity reduces the strength of the wood and causes corrosion of metal elements. This acidic environment is especially devastating in terms of the structure and coloration of paper and fabrics.

2. The absence of surface-active substances (surfactants) makes uniform and deep impregnation of the material.

3. Long-term temperature drying (1-3 weeks) is very energy intensive and leads to a strong increase in the value processed in such a way that material.

4. In the journey of this increased transport costs.

5. The preparation processes of composition and its use are environmentally unsafe, because in both phases is release into the atmosphere of acid vapor, acetic, phosphoric, perhaps, sulfuric or hydrochloric acids that are required for recovery and recycling and inevitably increases the value of the processed material.

Closest to the technical essence and the achieved effect of the present invention is a method of obtaining a flame retardant composition for treatment of cellulose-containing materials according to U.S. Pat. RF 2055857, IPC 6, FROM 09 TO 21/12, 1996. This method is a dry mixture of the LFA, or DAP, or their mixtures with urea in the ratio (1-2,3):1, moistening the mixture with water, alloying her at temperatures up to 120oTo obtain a product with MP. 102 to 106oC, cooling it with continued stirring until the grinding. At the stage of dry mixed in a composition can be introduced various surfactants, for example a mixture of alkyldimethylbenzylammonium with10-18in the alkyl, and ammonium halides such as ammonium chloride.

Consider the method according to U.S. Pat. RF 2055857 allows to obtain a fire-retardant agent with improved flame-retardant properties compared with other compositions obtained the composition, obtained by this method is a dry, non-dusting, Reconquista powder, environmentally safe storage and use. The composition readily soluble in water and is applied in the form of a 20-40% solution for the treatment of various cellulosic materials such as wood, fabrics, rugs and carpets.

However, consider for a stalemate. RF 2055857 fire-retardant composition is still insufficient flame-retardant properties (mass loss of the sample during the test - 15-19 wt.%).

The technical task of the present invention is to develop a method of providing flame retardant composition with a higher flame-retardant properties. The problem is solved in that in the method of obtaining a flame retardant composition comprising a dry mixture of the LFA, or DAP, or mixtures thereof with urea, moisturizing mixture, the introduction of surfactant, the fusion of the mixture when heated to 120oTo obtain a product with MP. 102 to 106oWith cooling and grinding the product under stirring, the surfactant is injected at the stage of fusion in the amount of 0.5 to 5.0% by weight of the dry mixture and fusion continue to receive product, 20% aqueous solution which has a pH of 5.0 to 6.2.

The introduction of surfactant at the stage of fusion of the mixture and not dry mixing the receipt of the product, 20% aqueous solution which has a pH 5,0-6,2, leads to the emergence of a new unexpected effect of improving the flame retardant properties of the synthesized compound.

The inventive method enables the production of ecologically pure composition with high flame-retardant properties. See tests for fire resistance of wood samples treated with this composition showed that the mass loss is 7-9 wt.%, that allows us to classify the processed material as nonflammable. Obtained by the present method, the composition is used in aqueous solution.

As a mixture of DAP and map in the present method uses, for example, a mixture with a mass ratio of the LFA:DAP=9:1 (map). As the surfactant used is preferably cationic surfactants, for example a mixture of alkylbenzyldimethylammonium with10-20the alkyl (I), a mixture of diallylmethylamine with17-20the alkyl (II), the mixture trialkylaluminium with7-9the alkyl (III), a mixture of alkyltrimethylammonium (bromides)10-16the alkyl (IV), a mixture of alchooxymethylolchlorbutane with10-18the alkyl (V), the mixture (acidication) methylmethanesulfonate with16-18the alkyl (VI), with Avow can also be used non-ionic surfactants, for example ethoxylated ALKYLPHENOLS with from 16 to 20 mol.%. ethoxylated units. The amount of added water during the hydration of the dry mixture before it is fused, preferably 3-5% by weight of dry components.

The inventive method is simple, single-stage, environmentally friendly, no harmful emissions and wastewater. Received the product very easy to use, because it is a non-dusting of loose powder, easily soluble in water (up to 60 wt.%); the humidity of the dry powder is not more than 2 wt.%.

The composition is an alloy of the LFA, or DAP, or their mixtures with urea and surfactant, has MP. 102 to 106oWith, which is different from the melting temperature as the original components and their dry mixes (MP. urea 132oWith; MP. The LFA 190oC; DAP decomposes without melting). It has a higher flame-retardant properties compared with the prototype and can be used in aqueous solution, optimally 20 wt.%. In addition, we use surfactants impart received additional properties - it has a pronounced fungicidal activity and along with giving the materials being processed trudnosgoraemostju protects and preserves the wood structure and coverage, as well as tissue paper from powerstat as follows.

The ammonium phosphate, which is used as the LFA, or DAP, or their mixture, is mixed with urea in dry form, preferably in a mass ratio of from 1.0 to 2.3):(1-3), respectively; the dry mixture is moistened with water, preferably in the amount of 3-5% by weight of the dry mixture, and melting. Fusion expediently carried out at a temperature not exceeding 120oTo obtain molten liquid mass. In the resulting melt enter the appropriate surfactant preferably in quantities of 0.5 to 5.0% by weight of the dry mixture and fusion continue to receive product, 20% aqueous solution which has a pH of 5.0 to 6.2; MP. it's 102 to 106oC.

In the present method can be used known additives target. As the target additives can be used, for example, ammonium halides such as ammonium chloride; sulfate or sulpham ammonium; polyphosphate sodium or potassium hydroxide; carbonates of sodium, potassium, ammonium, dyes, additives are introduced at the stage of dry mixing. Flame retardant in the form of an aqueous solution easy to cook in the workplace by simple dissolving the dry powder in water at room temperature. The working solution is applied on a protected surface by brush or spray to stop vetiva.

In experiments were used urea according to GOST 2081-92, MAF according to GOST 3771-74, DAP according to GOST 3772 -74, katamin AB TU 6-01-1816-74, map according to GOST 18918-95.

For a better understanding of the present invention, the following examples of implementation of the proposed method and testing of flame retardant properties of the resulting product.

Example 1.

In a horizontal reactor with a heated jacket and ribbon mixer with a capacity of 200 l load 50 kg LFA, 50 kg of urea are mixed and introduced 3 kg of water. The shirt serves vapor under a pressure of 2 ATM, providing the temperature in the mixer 120oC. when the mixture liquid state (melting), it is injected 0.5 kg (1) - ketamin AB and fusion continue to receive product, 20% aqueous solution which has a pH equal to 6.05. Served with a jacket water temperature of 25oWith continued mixing, the dispersed melt crumbs. Get the target product in the form of a grayish-white powder with MP. 104oC.

Test flame retardant properties of the resulting product is carried out as follows. Samples of wood, pine, size HH1 mm, conditioned to constant mass, kept in the working solution (20 wt.%) at room temperature for 2 h and dried at 70oM is determined with an accuracy of 0.1% according to the formulaM= (M1-M2)100/M1where M1and M2the mass of the sample before and after testing, respectively. For the test result arithmetic mean value is not less than 10 definitions.

Test results (valueM) establish a group of fireproof efficiency flame retardant: whenM<9% of the material is characterized as slow, with 9%<M<25% as a flame retardant. The results are given in the table.

Examples 2-9.

Obtaining a flame retardant composition and the tests were carried out as described in example 1. Variations of the composition of the initial mixture, the process conditions and the results of the test flame retardant properties shown in the table.

Example 10 (control).

In porcelain glass mixed in the dry state 50 g of urea and 50 g of the LFA, add 5 ml of water and 0.5 g PAVA (1). The mixture is heated on an oil bath to melt and maintained at 120oC for 30 min under intensive PE the comfort of the melt in the crumb. The final product has MP. 103oC.

From the product prepared impregnating an aqueous solution concentration of 20 wt. %; test flame retardant properties of the resulting solution similar to that described in example 1. The results are given in the table.

Examples 11-14 (control).

The process is conducted as described in example 10, but changing the appearance of ammonium phosphate, PAVA and the ratio of the components. Test flame retardant properties of the product carried out analogously to example 1. The results are given in the table.

Obtained by the claimed method flame retardant is suitable for the surface treatment or impregnation of cellulosic materials such as wood structural elements, mainly enclosed spaces and buildings, such as attics and ceilings, Museum interiors, also woven and nonwoven materials made from natural, synthetic or mixed fibers, for example, theatrical scenery, paper. The method can be easily implemented on a regular, widespread, standard chemical equipment.

Claims

A method of obtaining a flame retardant for cellulose-containing materials, and, introduction surfactants, fusing the mixture at a temperature of up to 120oTo obtain a product with so pl. 102 to 106oWith cooling and grinding the product under stirring, wherein the surfactant is injected at the stage of fusion in the amount of 0.5 to 5.0% by weight of dry ingredients and fusion continue to receive product, 20% aqueous solution which has a pH of 5.0 to 6.2.

 

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