RU2115545C1 - Agent "adbakh" for bioprotection of cellulose-containing materials - Google Patents

Abstract

FIELD: saw and wood working industry. SUBSTANCE: invention proposes bioprotective agent with respect to cellulose-containing materials from damage with wood-staining and mold fungi. This agent is a complex compound of the formula

Description

 The invention relates to means of organic origin used for the biochemical protection of cellulose-containing materials from blue stain and mold, in particular wood during its atmospheric drying for transportation with humidity higher than transport, and it can be used in sawmilling and woodworking industries.

 Known means of organic origin, with bioprotective properties in relation to cellulose-containing materials, which are compositions of organic ammonium fluorophosphate and / or diammonium phosphate and alkali metal fluorophosphate [1].

 The disadvantage of this tool is that its molecular solubility is small, the permeability of wood capillaries is low, since the surface tension of the aqueous solution is relatively high. Thus, the safety of samples of coniferous and deciduous species of sapwood against wood-staining and molds after exposure to 50 days is not more than 70%. This compound has a mainly bacteriostatic effect; delays the development or reproduction of microbes. The compound is toxic, belongs to substances of the 2nd hazard class, its aqueous solutions have a skin-irritating and pronounced skin-resorptive effect, causing dermatitis.

 The closest analogue to the described invention and adopted by the applicant as a prototype is a known agent of organic origin based on derivatives of thiophosphoric acid, in particular the preparation Basiment-475, produced in Germany by Desowg in the form of an emulsion concentrate based on a low toxicity thiophosphoric ester at a concentration of 2 - 3% in water [2].

 The drug protects not only from the action of wood and mold fungi, but also from beetles. However, a significant drawback of it is that it is capable of hydrolysis in the presence of moisture with the removal of an aliphatic or aromatic radical. Their insecticidal properties as a result of hydrolysis are almost completely lost. Storage of such preparations should be mandatory in the absence of moisture. In addition, the drug also cannot be stored in a metal container, since corrosion results in the formation of iron hydroxide, a gelatinizing drug, which makes it difficult to use. The drug is toxic, since thionic esters of thiophosphoric acid are easily oxidized. The surface safety of samples of coniferous and deciduous species of sapwood against wood-staining and molds after exposure for 50 days at a concentration of working solution of 3% is 55%, and at 5% it is 62%.

 This invention provides a bioprotection agent for cellulose-containing materials that is highly soluble in water, not hydrolyzed in moist environments, and has bactericidal and fungicidal properties against blue and mildew wood-coloring and wood-destroying fungi. This tool is safe for humans, its activity in time does not decrease, and the safety of wood samples after 50 days is 62% at a 3% concentration of the working solution and 82% at 5% concentration.

В промышленности предложенное средство получило название "АДБАХ". Получают "АДБАХ" следующим образом.The proposed tool relates to new derivatives of phosphonium compounds and is a complex compound of the structural formula

In industry, the proposed tool was called "ADBAH." Get "ADBAH" as follows.

Hydroxyethylidene diphosphonic acid (HEDPA) is charged into a steam jacketed reactor and, with continuous stirring, the temperature in the reactor is raised to 50 ^° C. Then, the di-substituted alkylmethylbenzylammonium chloride (BIOMIN) salt is gradually fed into the reactor. Moreover, in order to obtain a stable complex, the disubstituted salt of ammonium alkylbenzyl chloride is introduced in excess. The synthesis is carried out for 2 hours with a continuously working stirrer and at a temperature of 50 ± 5 ^o C.

В процессе производства определяют pH среды, проводят хроматографический анализ, по результатам которого определяют окончание проведения реакции. Потенциометрическим титрованием определяют кислотное число.The process goes as follows.

In the production process, the pH of the medium is determined, chromatographic analysis is carried out, the results of which determine the end of the reaction. Potentiometric titration determines the acid number.

 The proposed tool for bioprotection of cellulose-containing materials in production is called "ADBAH".

 Characterization of the initial products in the production of ADBAH.

 1. Oxyethylene diphosphonic acid (OEDPK) complies with GOST 12.1.007-76. HEDPK belongs to moderately hazardous compounds (111th hazard class).

2. Alkylbenzylammonium chloride contains at least 49-50% of the basic substance. Appearance - pasty mass of yellow color or gray-green color. The density of the solution is 0.96 - 0.97 g / cm, the pH of the aqueous solution is 6.6 - 7.0. The drug is moderately toxic, LD ₅₀ = 350 mg / kg for white mice.

The proposed tool is a viscous paste of light yellow color, having a slight smell of ammonia. Mass fraction of the main substance ≥ 98%, pH 8.8 - 9.5, temp. melting point = -198 - 199 ^o C, temp. freezing = -25 ^o C. Dynamic viscosity 20 (at 20 ^o C), 10 (at 40 ^o C), 6 (at 60 ^o C) cP. The solubility in g / 100 ml of the solution at 20 ^o C complete.

 The synthesis products of the proposed bioprotective agent were identified by chromatography on a UOG-1540 device (silica gel carrier modified with propylene glycol). The phase composition was studied using an X-ray diffraction study on a DRON-3M X-ray diffractometer with automatic processing of diffractometric patterns on a computer and obtaining diffraction patterns of interplanar distances. The product is isolated in dry form. To prove the content of the proposed complex, the dark-field method was used. The identification of bonds arising in the analysis of industrial samples of the agent was carried out by the method of IKS (Fourier spectrometer). Spectra corresponding to the final product were obtained.

 The effect of the proposed tool on wood was studied as follows.

 The tests were carried out in laboratory conditions. We used samples from sapwood of pine with a moisture content of 80 - 120%, measuring 5x15x180 mm (the last dimension along the length of the fiber). Samples were processed by immersion in impregnating solutions for 30 s. As a solvent used water.

 Samples were infected by the method of dipping into a suspension of spores of wood-staining and mold fungi.

As an inoculation material, a spore suspension of the following pure fungal cultures grown in test tubes on wort-agar medium was used:
wood stains: Pullularia pullulans, Phialophora fastigiata, Alternaria humicola, Cladosporium herbarium; and
mold: Penicillium meleagrinum, Trichoderma harcianum, Chactomum globosum, Aspergillus niger.

 After drying, the experimental samples treated with the proposed agent, to such an extent that there are no drops on the surface, were infected with a spore suspension. Why an aqueous suspension of spores is thoroughly mixed and poured into a vessel at the rate of 30 - 35 ml per sample. Samples are kept in suspension for 30 s and then they are dried to an initial moisture content of 80 - 120%. After that, the samples are placed in moist sterilized containers, in which the primary moisture content of the samples is maintained. On the 10th, 20th, 30th, 40th and 50th day of testing, a visual inspection of the samples is carried out and their surface fouling is evaluated by fungi as a percentage of the total area. According to the obtained results, the preservation of the samples is calculated, i.e. surface without fouling by mushrooms. Also using microanalyzers determine the distribution of the proposed tool for cross-section of wood after its impregnation.

 Indicators of the surface safety of the samples after different times (in days) depending on the concentration of the working solution of the proposed agent and prototype, as well as unimpregnated samples are presented in the table.

 From the table it follows that the reliability of the protection of wood samples is significantly higher when impregnated with the proposed tool than the tool of the prototype under equal conditions.

 Means "ADBAH" is well soluble in water, environmentally friendly, safe for the environment, can be used as an independent biocidal agent, or in combination with other additives. The wood after processing with “ADBAH” does not stain and does not change its physicochemical properties.

 The proposed tool relates to promising drugs for bioprotection of cellulose-containing materials and is especially recommended for the protection of lumber, when long-term action of the biocide is required.

Claims (1)

The complex compound of the structural formula

where R is a saturated hydrocarbon radical of normal structure,
as a means for bioprotection of cellulose-containing materials from damage by their wood-coloring and mold fungi.

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