Method for treatment of lignocellulose materials, in particular, wood and material prepared by this method

FIELD: wood materials.

SUBSTANCE: invention relates to a method for protection of wood providing to confer its hydrophobic properties for enhancing its longevity and stability of sizes. Invention describes a method for chemical treatment of lignocellulose materials, in particular, a wood lump. Indicated material is impregnated with a chemical agent containing hydrocarbon chains and this agent is chosen from mixed anhydrides containing the first hydrocarbon chain R and the second hydrocarbon chain R1 wherein R or R1 represents (C2-C4)-carboxylic acid, and R1 and R represents saturated or unsaturated (C6-C24)-fatty acid with exception mixed anhydride of acetic/benzoic acid. Indicated agent is useful for carrying out grafting based on a covalent bond in a great number of hydrocarbon chains with indicated materials. Grafting is carried out by the esterification reaction of indicated lignocellulose materials using a chemical agent chosen from organic anhydrides. Impregnation is carried out in the presence of a basic, neutral or weak acid catalyst and in the absence of catalyst also by immersion and irrigation in autoclave. Treatment is carried out at temperature from room value to 150°C but preferably from 100°C to 140°C. Also, invention describes an article based on lignocellulose fibers material, in particular, wood lump prepared by above described method. Proposed method provides preparing lignocellulose material, in particular, a wood lump with uniform fibers and smooth shape showing the absorption coefficient 3.5% and the swelling coefficient 3.5%.

EFFECT: improved method of treatment.

16 cl, 3 dwg, 3 tbl, 2 ex

 

The present invention relates to a method of processing lignocellulosic materials, in particular wood as well as material obtained by this method.

In particular, it relates to a method for protecting wood, allowing you to give it a hydrophobic character to improve its durability and dimensional stability.

It is known that the natural state of the wood or, more precisely, wood fiber in contact with a humid atmosphere, tend to absorb water. This absorption of water is accompanied by swelling.

Removal of this water can be used for drying. However, although the stage of drying and allows you to remove the water from the wood, it does not change the natural hydrophilic character of the latter, so that the piece of wood when placed in a humid environment can again reabsorbable water removed during drying.

To reduce or even eliminate the hydrophilic nature of wood and giving it a long-term dimensional stability (usually for a period of about ten years) developed processing technology.

They can be divided in two large families with different physical methods of heat treatment (typically at temperatures above 150°C and methods physico-chemical treatment, usually at temperatures below 120°C.

In the present invention consider the Xia methods of physico-chemical treatment.

Of these physico-chemical treatments known in particular from a number of publications Arni et all., (Arni, 1961); Matsuzaki et all., ways to synthesize mixed esters of triperoxonane environment. These methods are not applicable on an industrial scale because of the need for the use of toxic solvent and catalyst.

Additional research conducted on wood sawdust, showed that the esterification in the presence of a strong acid catalyst (add to its acidity) allows you to give these filings hydrophobic character. This research was devoted to the following publication Vaca-Garcia C;, Borredon M.E, 1999, Solvent-free fatty acylation of cellulose and lignocellulosic wastes. Part 2: reaction with fatty acids, Bioresource Technology, 70, 135-142.

Significant disadvantages of this method, requiring the presence of an acid catalyst, are in the weight loss sawdust, and this weight loss is a result of the destruction of the components of sawdust biopolymers. You can also notice a change in the color of sawdust after processing.

The technology, similar to the previous one, unbearable on a piece of wood. Indeed, it was found that the molecules of hemicellulose and cellulose, partially hydrolyzed, resulting in decrease in molecular weight due to the formation of oligomers, as well as the deterioration of mechanical properties and appearance clicks the spent piece of wood.

The present invention aims at eliminating these disadvantages by using the proposed method, which gives the wood a hydrophobic character, while ensuring dimensional stability in time without causing any cracking, tremendously, schisms, no color change.

Thus, an object of the present invention is a method of chemical treatment of lignocellulosic materials, in particular, at least one piece of wood, characterized in that said materials are impregnated with a chemical agent containing hydrocarbon chain, and the specified agent is chosen from mixed anhydrides with the exception of mixed anhydrides of acetic acid/benzoic acid, and the specified agent is suitable to provide vaccinations due to the covalent bond of many hydrocarbon chains for these materials.

This ensures improved protection on the surface and in the center of the lignocellulosic material, in particular wood, by changing its hydroxyl functional groups.

In preferred embodiments of the invention can additionally be used one and/or more of the following provisions:

- vaccination is carried out by esterification of these lignocellulosic materials by chemical agent selected from the PR is hanicheskih anhydrides,

the treatment is carried out at a temperature from room temperature up to 150°C, preferably from 100 to 140°C

organic anhydride is a mixed anhydride,

mixed anhydride contains the first hydrocarbon chain R and the second hydrocarbon chain R1,

- R represents a C2-C4-carboxylic acid, a R1represents a saturated or unsaturated With6-C24fatty acid,

- R1represents a C2-C4-carboxylic acid, and R represents a saturated or unsaturated With6-C24fatty acid,

mixed anhydride is a mixed anhydride of acetic acid/octanoic acid,

the impregnation is carried out in the presence of a basic catalyst,

the impregnation is carried out in the presence of a neutral catalyst

the impregnation is carried out in the presence of a weak acid catalyst,

the impregnation is carried out in the absence of catalyst,

the impregnated lignocellulosic materials are dipped,

the impregnated lignocellulosic materials is carried out by irrigation,

the impregnated lignocellulosic materials is carried out in an autoclave,

- processing method carried out on a piece of wood, the base of which is selected in particular from oak, pine, spruce, curupixa, eucalyptus.

According to another aspect of izopet what of it also applies to the piece of wood, processed according to the above method and characterized in that the lignocellulosic fibers are homogeneous and have a smooth appearance.

In preferred embodiments of the invention can optionally use one and/or more of the following provisions:

is the absorption coefficient of the treated lignocellulosic fibers substantially close to 3.5%,

the ratio of swelling of the treated lignocellulosic fibers substantially close to 3.5%.

Other characteristics and advantages of the invention will be revealed in the following description of one of the forms of its implementation, is presented as a non-restrictive example, and the attached drawings.

Figure 1 is an image obtained scanning electron microscopy (SEM) of a sample of raw wood; this sample can be taken as control.

Figure 2 is an image obtained with the scanning electron microscopy (SEM) of a sample of wood held processing method, which is the object of the invention, in the presence of a strong acid catalyst.

Figure 3 represents another picture, obtained by scanning electron microscopy (SEM) of a sample of wood held processing method, which is the object of the invention, in the presence of a strong sour the aqueous catalyst.

According to a preferred variant of the method, which is the object of the invention, this method consists in impregnating lignocellulosic materials, such as, in particular, as at least one piece of wood with a chemical agent containing hydrocarbon chain, and the specified agent is suitable to provide vaccinations due to the covalent bond of many hydrocarbon chains for these materials.

Under hydrocarbon chain understand any heteroaromatics, heteroaromatic, aliphatic or aromatic chain.

This impregnation is carried out at a temperature from room temperature up to 150°C, preferably from 100 to 140°C.

This chemical agent is chosen from organic anhydrides, preferably mixed anhydrides.

Before impregnation stage chemical agent specified lignocellulosic materials (for example, at least one piece of wood) conduct a stage of preparation of the mixed anhydride.

According to the first method: based on the carboxylic acid and ether carboxylic acids according to the following reaction:

According to a variant of the first method, consisting in the replacement of the provisions of the R and R1

According to the second method: based on the carboxylic acid and salts carbon is howling acid according to the following reaction:

According to the third method: based on the anhydride of the carboxylic acid with a straight chain fatty acid according to the following reaction:

The radicals R, R1represent aliphatic chains of different length. As a non-restrictive example, the length of R is less than the length R1.

R denotes, for example, With2-C4-carboxylic acid (acetic, propionic or butyric), whereas R1represents a saturated or unsaturated With6-C24fatty acid (e.g., nylon, octane or oleic).

Mixed anhydrides can be used in pure form or in mixtures and in this case can be derived from mixtures of different carboxylic acids, which carry out the synthesis of the desired mixed anhydride.

Using the mixed anhydride obtained according to at least one of the above methods, carry out the impregnation of the piece of wood in such a way as to carry out the inoculation of the mixed anhydride (e.g. acetic anhydride/octanoic acid) to the specified piece of wood, and vaccination is the esterification of wood according to the following reaction:

Or, on the contrary, in regard to the role of R and R1

Can also be used other methods of esterification considered according to the following reactions:

Based on carboxylic acid; this reaction is fast, but a significant disadvantage is the evolution of HCl.

As an example, the acid chloride acid selected from octanoylthio, acetylchloride.

Based on tseten; but used in this case, the reagents are expensive, which reduces industrial interest.

As an example, this reaction can be combined using, for example, octanoylthio.

Based on carboxylic acids; however, this reaction has a low reactivity and requires the use of co-reagents: pyridine, DCC, TsCl, TFAA (DCC: N,N-dicyclohexylcarbodiimide; TsCl: p-toluensulfonate; TFAA: triperoxonane anhydride)

As an example, the carboxylic acid is chosen from acetic acid, octanoic acid.

Based on esters of carboxylic acids (for example, methyloctanoic, acetate); it can be noted, however, that when R consists of CH3highlighted is methanol (toxic).

Mixed esters of wood can be obtained either

in one stage by mixing Reagan is s, selected among the above;

or in stage 2,

either twofold repetition of one and the same type of reaction,

or the two reactions two different families.

In addition, according to one of the features of the invention these esterification reaction can take place in the absence of catalyst or in the presence of a basic or neutral catalyst (such as calcium carbonate, sodium carbonate, potassium carbonate, salt fatty acids...), or with a weak acid catalyst, or with a strong acid catalyst, whose adverse effects on wood minimize, using a very weak concentration.

The following are examples of implementation of the method according to the invention.

Example 1: To 1 mole of octanoic acid was added 1 mol of acetic anhydride. The mixture is heated with stirring at a temperature of 140°C for 30 minutes. A piece of wood the size 10×10×10 cm are immersed in the reaction mixture and heated at 140°C for 1 h the mixture is allowed to drain with a piece of wood and the latter is dried in a ventilated oven.

Example 2: To 1 mole of octanoic acid was added 1 mol of acetic anhydride. The mixture is stirred at room temperature for 60 minutes. A piece of wood the size 10×10×10 cm are immersed in the reaction mixture for 5 minutes, the mixture is allowed to drain. For the eat the piece of wood placed in an oven for 1 h at 120° C.

A significant advantage of the present invention is that use mixed anhydride of plant origin, which is non-toxic in contrast to compounds of petrochemical origin.

This particular choice facilitates industrial implementation of the invention, since it simplifies the process, with the intention of protecting the environment.

Regardless of the method of processing characteristics of the processing, you can finda posteriorion lignocellulosic material (in our case on a piece of wood).

Can be used various techniques to characterize the processing, which was subjected to a lignocellulosic material, namely the presence of different hydrocarbon chains, linked through ester functional group, and the presence or absence of a catalyst (and its type).

The way to determine the presence of hydrocarbon chains, is in the handling of sample obtained from a piece of wood, NaOH solution for hydrolysis of the ester functional groups and conversion of the hydrocarbon chain in the carboxylic acid. The latter then identify by conventional methods of chromatography, such as HPLC, gas chromatography, etc.

An example of such technique is getting complex mixtures is Firov, for example acetates and octanoate lignocellulosic material, on the basis of a piece of wood or lignocellulosic material, the hydroxyl functional groups which were etilirovany at least two different hydrocarbon agents.

This mixture of esters can be characterized as follows: a sample of wood or lignocellulosic material treated with the claimed method, milled to obtain a particle size of at least 80 mesh, and then placed in a flask containing an aqueous solution of ethanol (70%). After stirring for at least 1 h add a sufficient quantity of an aqueous solution of NaOH (0.5 M) and continue stirring for 72 h for the complete saponification of the ester functional groups. After filtration and separation of a solid residue liquid is acidified to pH 3 with aqueous HCl (1 M) for the conversion of hydrocarbon compounds into the corresponding carboxylic acid. The liquid is then analyzed by gas chromatography (CPG) or high performance liquid chromatography (HPLC) for the separation and identification of various carboxylic acids corresponding to those present in the treated wood or lignocellulosic material ester functional groups.

Below are techniques to determine the type is utilizator.

So, the first technique consists in determining the amount of extractables. This technique allows to observe the effect of different treatments on the extracted wood substances initially present or resulting in the destruction of wood). Processed and then chopped the wood is subjected to extraction using several solvents with different polarities: water, ethanol, acetone and cyclohexane. Extraction is carried out using Soxhlet apparatus.

The following table presents the quantities of substances extracted from samples treated wood after extraction in Soxhlet with different solvents.

Weight loss (%)after extraction
WaterEthanolAcetoneCyclohexane
Without catalyst14,811,912,26,3
The main catalyst17,116,210,61,8
A strong acid catalystto 25.321,719,04,8

As can be seen from the table, regardless of the extraction solvent, these results confirm the visual impressions: processing in the presence of a strong acid catalyst (0,3 mol.% H 2SO4), which is the most powerful destroyer of leads at the end of the reaction to the formation of the greatest amount of extractable compounds. When significant quantities of strong acids (0,3 mol.%) a piece of wood darkens and has a tendency to destruction and the appearance of external faults.

Microscopic examination shows that the cell walls of fibers damaged by acid catalyst.

So, comparing Figure 2 with Figure 1 from a qualitative point of view, we can state that the surface of the wood seems to be polished by using the processing carried out; the wood surface is homogeneous. Woody (lignocellulosic) fibers visible in the microscope, appear to be intact compared with the fibers in figure 1. On the one hand, the product seems to be subjected to the kind of the Etchant surface, which, however, allowed to homogenize the surface through vaccination. Indeed, the grafted chain protects fiber, which makes them indistinguishable under the microscope.

Similarly, figure 3 lignocellulosic fibers seem to be naked. The presence of the product is much less clear than in the previous case (Figure 2); this is logical, because the picture shows the inner part of the block processed by the method according to the invention. Stratification due to either processing or probably breaks the fibers while allowing the offering.

From a quantitative point of view, the magnitude of absorption and swelling of the treated and untreated lignocellulosic fibers are presented in the following table.

Raw fiberThe processed fiber
Absorption,%163,5
Swelling,%6,53,5

The second technique is the analysis of the components of wood. Depending on the type of environment in which the treated wood, not all biopolymers wood subjected to the same destruction. The composition of the treated wood may, therefore, vary depending on the processing. This technique is called ADF NDF; it allows you to learn the proportions of cellulose, hemicellulose N, lignin L, inorganic substances MM.

The following table summarizes the results of the analysis of the composition of oak wood, processed mixed acetic-octane anhydride with various types of catalysts. Esterified samples were subjected to saponification in accordance with a written analysis of mixed esters of wood, then were washed by extraction with water using a Soxhlet apparatus, and then subjected to analysis by technology ADF NDF. This technology (Acid Detergent Fiber, Neutral Detergent Fiber) is described in the works of the VAN SOEST P.J. and WINE R.H. Determination of lignin and cellulose in acid-detergent fiber with permanganateJ. Ass. Office. Anal. Chem.51(4), 780-785(1968).

The nature of the treatmentRolled-jamExtra-geremie matter (%)Cellulose

(%)
Hemi-cellulose

(%)
Lignin

(%)
Different

(%)
Ash
Raw wood-5,050,917,620,5of 5.40,6
A strong acid catalystH2SO4< / br>
to 0.3 mol.%
22,449,714,78,54,40,3
The main catalystNa2CO3< / br>
to 0.3 mol.%
16,940,616,420,1the 5.70,3
Without catalyst-12,541,4of 17.517,110,80,7

Thus, this analysis allows to distinguish treatment with a strong acid catalyst from the declared types of processing. Indeed, there is a significant exponential decrease in the amount of lignin and hemicelluloses. In addition, the number is the amount of extractable water in Soxhlet substances is the greatest.

1. The method of chemical treatment of lignocellulosic materials, in particular, at least a piece of wood, characterized in that said materials are impregnated with a chemical agent containing hydrocarbon chain, and this agent is chosen from mixed anhydrides containing the first hydrocarbon chain R and the second hydrocarbon chain R1where R or R1represents a C2-C4-carboxylic acid, and R1or R represents a saturated or unsaturated With6-C24fatty acid, with the exception of the mixed anhydride of acetic acid/benzoic acid, and the specified agent is suitable for the implementation of vaccinations due to the covalent bond of many hydrocarbon chains for these materials.

2. The method according to claim 1, wherein the inoculation is carried out by esterification of these lignocellulosic materials by chemical agent selected from organic anhydrides.

3. The method according to claim 1, wherein the treatment is carried out at a temperature from room temperature up to 150°C, preferably from 100 to 140°C.

4. The method according to claim 2, characterized in that the treatment is carried out at a temperature from room temperature up to 150°C, preferably from 100 to 140°C.

5. The method according to claim 1, wherein the mixed anhydride is a mixed anhydride of uksosn the th/octanoic acid.

6. The method according to one of claims 1 to 5, characterized in that the impregnation is carried out in the presence of a basic catalyst.

7. The method according to one of claims 1 to 5, characterized in that the impregnation is carried out in the presence of a neutral catalyst.

8. The method according to one of claims 1 to 5, characterized in that the impregnation is carried out in the presence of a weak acid catalyst.

9. The method according to one of claims 1 to 5, characterized in that the impregnation is carried out in the absence of a catalyst.

10. The method according to one of claims 1 to 5, characterized in that the impregnated lignocellulosic materials are dipped.

11. The method according to one of claims 1 to 5, characterized in that the impregnated lignocellulosic materials is carried out by irrigation.

12. The method according to one of claims 1 to 5, characterized in that the impregnated lignocellulosic materials is carried out in an autoclave.

13. The method according to one of claims 1 to 5, characterized in that it is carried out on a piece of wood, the base of which is selected in particular from oak, pine, spruce, curupixa, eucalyptus.

14. The product on the basis of the fibers of the lignocellulosic material, in particular a piece of wood obtained by a method according to one of the preceding paragraphs, characterized in that the lignocellulosic fibers are homogeneous and have a smooth appearance.

15. The product on the basis of the fibers of the lignocellulosic material, in particular a piece of wood obtained by a method according to one of claims 1 to 13, characterized in that the absorption coefficient is substantially close to 3.5%.

16. The product on the basis of the fibers of the lignocellulosic material, in particular a piece of wood obtained by a method according to one of claims 1 to 13, characterized in that the coefficient of swelling significantly close to 3.5%.



 

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1 tbl, 5 ex

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11 cl, 5 tbl

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FIELD: wood materials.

SUBSTANCE: invention relates to a method for protection of wood providing to confer its hydrophobic properties for enhancing its longevity and stability of sizes. Invention describes a method for chemical treatment of lignocellulose materials, in particular, a wood lump. Indicated material is impregnated with a chemical agent containing hydrocarbon chains and this agent is chosen from mixed anhydrides containing the first hydrocarbon chain R and the second hydrocarbon chain R1 wherein R or R1 represents (C2-C4)-carboxylic acid, and R1 and R represents saturated or unsaturated (C6-C24)-fatty acid with exception mixed anhydride of acetic/benzoic acid. Indicated agent is useful for carrying out grafting based on a covalent bond in a great number of hydrocarbon chains with indicated materials. Grafting is carried out by the esterification reaction of indicated lignocellulose materials using a chemical agent chosen from organic anhydrides. Impregnation is carried out in the presence of a basic, neutral or weak acid catalyst and in the absence of catalyst also by immersion and irrigation in autoclave. Treatment is carried out at temperature from room value to 150°C but preferably from 100°C to 140°C. Also, invention describes an article based on lignocellulose fibers material, in particular, wood lump prepared by above described method. Proposed method provides preparing lignocellulose material, in particular, a wood lump with uniform fibers and smooth shape showing the absorption coefficient 3.5% and the swelling coefficient 3.5%.

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16 cl, 3 dwg, 3 tbl, 2 ex

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