JPS59218807A - Method of improving and treating woody material - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed Description of the Invention] The present invention is capable of manufacturing with high productivity a modified wood material that can eliminate the defects of wood and have a durability comparable to that of wood H. This relates to the modified 7'1 processing lJ method on the tree'f1 side.

Wood and processed wood i"t l: 4-i' d wood (Δ
Wood materials such as decks and wood chips are light Lithium and strong, and have unique physical properties and a sense of purity.They are used not only for construction and furniture, but also for a wide range of other applications. There is.

However, in 4R and -R, wood materials are susceptible to erosion by various fungi and insect damage such as termites, and are susceptible to disease and decay, and in recent years, living environments with high airtightness and heating equipment have become widespread, and the wood absorbs carbon.・h'
l iBt J There is a tendency to cause warping, twisting, and deformation of the expansion cage as a result of sagging.In order to improve the former problem above, impregnation treatment with a disease preventive agent such as creosote oil is generally performed. However, it has disadvantages such as its odor, which limits the places where it can be used, and the fact that it further increases the flammability of the water.

On the other hand, to improve the latter problem, water-based materials are treated with 1'il acid anhydride to acedelize some of the hydroxyl groups in the wood.

0113G O \ Wood -ON 10/ C1-1 CO ↓ Wood -OCOCl-1: + i-CI-1
c 6 o +-+ The above acetic acid is A-L? when using a sulfuric acid catalyst. Experimentally, it has been shown that 1T promotes the monomerization reaction.
1' recognized and J3 reaction on fat FI12 If'
iii'l Although it is said that there is no problem even if the salts are treated with a catalyst, it is preferable to treat the salts by the method 1, in which the salts are catalyzed. It has been confirmed that acetic acid inhibits the reaction of nl acid anhydride that appears in the hydroxyl group of wood 714A, and if an effective modification treatment is performed, the following problems will occur. -0 Immediately (1) If the reaction solution is used repeatedly, is a large amount of free material released in the reaction solution? 11 acid is generated, and the free acetic acid inhibits the reaction between the wood and acid anhydride, resulting in a slow reaction rate and a long processing time, making it difficult to reuse the reaction solution. and 41s, 1
聚41-Industrial large<f, H woody month Iy modified 7゛(processing J
It is not economical to do so because a large amount of reaction solution is wasted.

(2) If you use the reaction solution repeatedly and cover it, will it be 1 in the reaction solution? Since a large amount of ^1 acid becomes present, the wood 71 material swells and deteriorates.

In addition, since the wood (A is kept in an absolutely dry state) is hard to handle, it is preferable to treat it with a moisture content of the same level as the normal air-drying process. If the moon is put into the reaction solution while still retaining water, it will be 1! ! (Water 1N
There was a problem in that the +acid reacted with the moisture in the wood (converting it to n-acid and fractionating it in large quantities required 100 ml of water).

Therefore, the modification effect of conventional wood 7'i4Δ by aredelization treatment has been investigated in various ways, and although it has been recognized in experiments, it is difficult to process it industrially11. Tree!,: Treated water Ki 4 for practical use
It took a long time to mass produce A.

The present invention has been made in view of the above-mentioned problems in the acetylation treatment of wood. ,': Anhydrous acid-resistant reactant is infiltrated into the reaction wave and subjected to acetylation treatment, and the selected Nf n+ acid salt reacts to form a double salt. In order to prevent the formation of a solution and the increase of free acetic acid in the reaction solution, free nl M:'
It is characterized by preventing reaction inhibition caused by J as a by-product of M, maintaining the viscosity of the reaction solution, and preventing deterioration of water quality materials caused by J in acetic acid. After or during the reaction treatment, a portion of the reaction liquid is collected into the reactor and cooled, and then it is released as crystals of double n. C reaction 1137 by removing one component of double salt from 1k
4. The reused double salt was crystallized, precipitated and recovered. , the salt condensation product is medium (1, I L'T i'liσr11
2. )Dolly)Things-(They are mixed in the above reaction solution^!
lI! 2 As salt? For Ij publication, wood'? An economical 11-rich wood material modification process that can recycle the free rll acid produced as a by-product in the acedelization process for 1 wood for 6 effects. I! 1-
It provides the J method.

The method of the present invention will be explained in detail below.

First, add acetate (2
) is immersed in the reaction solution (3) containing 1Iiii acid anhydride as a reactant.

As the acetate (2) to be mixed in the above reaction solution, for example, sodium acetate, potassium ester, etc. is used.

This 1VFt salt is extremely easily soluble in 101 acids, but is insoluble in acetic anhydride, so that the acetic anhydride level of the reaction solution can be reduced to 11t l-U, and J, woody Since the material does not inhibit the reaction of acetic anhydride, it does not lower the IIS 11 degrees of the reaction solution even if it is mixed into the reaction solution in advance.

In addition, the above reaction liquid speeds up the reaction with the water-based material.It is not necessary to infiltrate the interior of the wood material into the surface layer of the water-based material. It can be converted into acedel.

This n; 1J wood ¥ 1 material aletylation rate (, 1, 11 method stability, durability, water absorption, etc. of wood H to avoid discoloration, acepulization treated water 71H medium weight increase rate after treatment is 15%
It is desirable to do it so that the above is achieved.

If only the surface layer is chilled, the water quality material should be treated so that the weight increase rate of the surface layer is 15% or more.

At this time, free acetic acid is produced as a by-product in the reaction solution due to the acedelization of water M)3 in the wood, but since acetate is present in the reaction solution, the 3r1 released acetic acid and nl salt resistance is 2C113COON-ICt-13COONai'
Cl-13COONa m 2Ct-h CO'OH represented by the formula μJ forms a double salt solution with weak bonds, and rr is present in the reaction solution.As a result, Above a certain concentration of free acetic acid, there is no decrease in the reaction solution speed.

That is, if the reaction process is repeated with free acetic acid in the reaction solution '/l (i:μ), MfA acetic acid 117Ia
The acetylation reaction is inhibited by the increase in the acetylation reaction, and even if 01 acid anhydride is added to the reaction solution in the same amount as the acetic anhydride consumed in the reaction, it is difficult to achieve the same treatment effect as the first time. With the method of the present invention! Aretylation treatment in the presence of IV salt 111I! Since free 111 acid is produced as a by-product and is present in the reaction solution in the form of a 6-stage salt, the consumed amount of acetic anhydride is added to achieve the same treatment method as the initial one.

The reaction solution subjected to the reaction treatment in this way can be used as it is by adding the acetic anhydride reduced in the reaction, but if the repeated use is reduced, a large amount of step salts will be present in the reaction solution. Where is the sea urchin reaction solution? [! (In order to reduce the iL force, if the J exceeds -Tm, it will react after the reaction is completed or during the reaction.) A portion (3') of 1 is added to a cooling device, etc. (4) in 11 L for 12 minutes. Cool it using
The double salt is separated from the reaction wave without crystallization, and the reaction 11R (3'') from which the μ, 1!2 salt is removed can be recycled to the reaction tank (5).

In other words, the double salt formed by the combination of acetic acid and acetate is 10, and thus 10 is forced out of the reaction solution. ! The 2-salt crystal is directly used as hRF.
If f is kept, the acepulization reaction will be repeated, resulting in
When a certain amount is reached, it can cause adverse effects such as clogging the circulation system of the reaction tank, etc.
), Jru.

In addition, the double salt crystals separated and collected (after recovery, the double salt crystals are neutralized with 1-11 hydroxide or hydroxide) to remove moisture, and are mixed into the reaction solution to form a reflux-resistant salt. 01
It can be used cyclically as an acid salt, and the reaction solution can be used without waste to carry out industrially productive modification of wood materials.

In addition, the order of acetate mixed into the reaction solution depends on the suspension of the treated wood, and the reaction rate of free acetic acid produced as a by-product in the reaction tank, etc. If you keep it mixed, J, ku,
You may add more depending on the state of dissolution.

Examples of the method of the present invention (Ij J) and comparative examples are shown below.
After drying, catalyst-treated wood 11 was obtained.

Next, the water strip described in J. was immersed in a reaction solution (500 g) of acetic anhydride heated to 110"C-120°C for 30 minutes.
After reacting for minutes, wash with water and dry to obtain an aletylated plate with an apparent acetylation rate of about 25%.

Qt in the reaction solution after reaction I2!2 Fuchika IJ treatment f) I
It was 2% higher than J.

- Comparative Example 2 - Similarly to the reaction solution used in Comparative Example 1, the irrigation deck used in Comparative Example 1c was added and subjected to acetylation treatment. tree 4
A Ili temporary is added and -C alledylation reaction is carried out%
People who have fallen into two.

- Example ~ No. 1 ((Water and acid resistant reaction solution <500 CI) and acetic acid solution
-The acetylation rate of the heating plate was measured at 120'C with 10g of aluminum (10g) mixed in advance, and the noacetylation rate (f
The increase in the amount of fi (IJ) was approximately 24%' (・There was almost no decrease in the treatment effect.

At this time, the MI II mixed into the reaction solution was ``C'' due to the presence of a double salt solution of the 61-acid salt in the reaction solution.

Next, take out about half of the reaction solution and pass it through the cooling tube for 20 minutes.
'W cooled to C, ^1 salt? 2 J = Approximately 1 liter of water is circulated into the reaction tank to precipitate the crystals and separate the compound Jjuf from the reaction solution.
0 g of the puttrium acetate crystals were mixed into the reaction tank.

When the Holo L11 plate was immersed in the readjusted reaction Hk and treated again, there was no decrease in the reaction rate, and the C-aretylation rate was 24 in the same place as the first time.
96 modified wood veneers were obtained. In addition, when we compared the strength of the acetylated pressed single plate obtained by this method and the acetylated pressed deck obtained in Comparative Example 2, the pressed deck plate obtained in Comparative Example 2 had an expansion i1'71 L-1. Although the wood veneer used to be brittle and easily broken, this method does not reduce the strength of the wood veneer. Since free acetic acid is generated as a by-product during the reaction, the acetic acid reacts at the same time to form -C double salt. Since the reaction between wood and acetic anhydride does not cause any damage or deterioration of the wood, it is possible to efficiently form modified wood with stable properties at all times. .

In addition, reaction process F[! In 112, in addition, in the reaction process (take out -ψ1; of the reaction solution from 11 and cold AI]), crystallize and separate the above ?!2 salt,
Since the reaction solution is recycled to the reaction tank again, there is no need to waste the reaction solution, and the reaction solution can be used for convenience.

Furthermore, 1. : By neutralizing the compound JAa filtration, a new fitlIQ salt was obtained, and this was used again for the 0Y salt mixed in the reaction solution to the PJJ that was produced as a by-product during the treatment. IrJ! Q is t)F1(((Unavailable K・reprocessing■) It is the same as using C in the line. This is a clear diagram showing the flow of the manufacturing process.

(1)... Tree'f1(Δ, (2)... Acetate, (3
)...Reaction liquid, (5)...Reaction tank, (6) Double salt crystal.

Claims (3)

[Claims] (1) A wood-side modification treatment method characterized by performing an acedelization treatment by immersing a wooden material in a reaction solution containing n1 acid anhydride mixed with acetate as a reactant. (2) Wooden materials, rll 11j! Acetylation treatment is carried out by mashing 27< in a reaction solution containing salt-mixed anhydrous 1-acid as a reactant, and a part or all of the reaction solution after the treatment is poured into a cold IJ to obtain a complex of acetic acid and 1-acid. A method for modifying wood materials characterized by recovering double salts by precipitating salts. (3) Wooden material mixed with vinegar and salt 2+!
+ Immersion in a reaction solution containing aqueous acetic acid as a reactant - (performing acetylation treatment)! I! Part or part of the reaction solution after
) is cooled to precipitate a double island of acetic acid and 61 acid salt and collect the double salt, and then the double salt is neutralized to form an acetate,
The acetate resulting from this neutralization is added to the above reaction solution and reused, which is considered to be a characteristic of a wood material modification process. P method.