DE2410746A1 - METHOD AND MEANS FOR BINDING LIGNOCULLULOSE MATERIAL - Google Patents

Description

CANADIAN PATENTS AND DEVELOPMENT LIMITED ■ Ottawa, Ontario, Canada

Method and means for binding lignocellulosic material

Priority: USA dated March 6, 1973 No. 338 562

A 0.9 837/0869

The invention relates to a composition and a method for binding lignocellulosic materials, in particular a composition comprising a concentrate of lignosulfonate or sulphite waste liquor and a mineral acid contains, as a binder for chipboard.

The most commonly used adhesive binders for chipboard are urea-formaldehyde and phenol-formaldehyde condensates. Conventional Trusses make up a large part of the total material cost of particle board. It is therefore easy to see that the "use of a relatively cheap material such as lignosulfonate or sulfite waste liquor as Binder would be desirable.

There are numerous proposals for the use of sulphite liquor as an adhesive binder for particle board, but none of these proposals has been entirely satisfactory, particularly with a view to reducing the overall production costs of particle board. A number of previous proposals have included the chemical modification of the spent sulfite liquor prior to its use as a binder, and most modified resins contain less than 50 % spent sulfite liquor solids. The actual cost of producing the modified waste liquor is not appreciably less than that of the commercial phenolic and urine-formaldehyde-based substances.

Canadian patent 74-3 861 describes a method for using sulphite waste liquor for chipboard, the waste liquor (a solution with 50 % solids content) being adjusted to a pH of about 3 with acetic acid. However, in order to achieve a satisfactory bond, it is stated that two stages of curing of the binder are necessary. In the examples of this patent, the first stage involves pressing a 12 mm (1/2 inch) plate at 185 ° C

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■ '- 3 -

(365 ⁰ F) for 30 minutes. In the zx ^ nits stage, the plate is introduced into an autoclave and heated under pressure to 195 ⁰ C (383 ⁰ F) for 80 minutes. In this process, the gate part of using the much cheaper waste liquor as a binder is largely offset by the cost of the long press time, ie 30 minutes instead of about 8 minutes for panels made with phenol-formaldehyde binder, and considerably longer for the autoclave step. ·

The aim of the invention is therefore a composition for binding of lignocellulosic materials comprising lignosulfonate treated to reduce pH, and a binder for lignocellulosic materials which contains lignosulfonate and a mineral acid in combination to form a To achieve binder in dry powder form.

Another object of the invention is a method for producing an adhesive binder for lignocellulosic materials, the Contains lignosulfonate, and in particular a method for binding lignocellulosic materials using Lignin sulfonate.

Accordingly, the invention also leads to a method of manufacture of chipboard using lignosulphonate, the pressing time being comparable to conventional pressed particle board using conventional binders, as well as the production of particle board using Lignosulfonate, the quality of which is suitable for outdoor use, as well as the achievement of particle board, the ligninsulfonate and which are easily produced using the existing technology of chipboard manufacture can be.

Finally, the invention relates to the use of sulphite waste liquor as a source of lignosulphonate for a Zlebinder.

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According to one aspect of the invention there is a composition for binding lignocellulosic materials supplied by concentrated lignosulfonate is treated to its To reduce the pH to less than 2, preferably to about 0.2 to about 1.5 »measured as a 50% solution of the lignin sulfonate s.

The most economical method of lowering the pH seems to be achievable by adding a steric acid. However, the pH value can also be lowered by any other method, whereby the cations are replaced by hydrogen ions be replaced, for example by electrodialysis.

The insoluble salts are preferred when they are added precipitate from acid, removed.

The most convenient I-form for the binder composition is believed to be the dry powdered form obtained by spray drying a mixture of sulphite waste liquor and Mineral acid is available.

In a special embodiment of the invention, the adhesive binder is subjected to a heat treatment. The heat treatment can be applied to the lignosulfonate before or after the addition of a mineral acid.

According to a further aspect of the invention, particle boards are made from lignocellulose particles, a concentrate of lignosulphonate and a mineral acid.

In one method, a mineral acid is first mixed with wood particles, and the acid coated particles are then mixed with dry, powdered lignosulfonate or spray-dried sulfite waste liquor. It will be a train formed with the mixture, which is then at a temperature of

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about 150 ⁰ G (300 ⁰ P) or more is hot-pressed.

According to another procedure, an adhesive binder containing lignosulfonate and a mineral acid is prepared prior to mixing with the particles. In one form, the binder contains concentrated lignosulfonate and mineral acid in liquid form. In another form, the combination of concentrated lignosulfonate and mineral acid is spray dried, resulting in a dried powdered binder. If the adhesive binder is mixed with the particles in liquid form, it may be necessary to "dry the mixture" to achieve a moisture content of preferably between 6 and 12 % . The web of particles and binder can be hot-pressed around the panel to solidify and harden in one operation, or it can be hot-pressed to solidify and partially harden the chipboard, and then post-hardened at an elevated temperature.

The composition for binding lignocellulosic material preferably comprises lignosulfonate in proportions which are equivalent to at least 2 percent by weight solids, based on the weight of the lignocellulosic material, and a mineral acid in proportions that are two to 20 percent by weight, measured as concentrated sulfuric acid, by weight on lignosulfonate, are equivalent. 2 to 20 % concentrated sulfuric acid are etvia. equivalent to a pH of 2 to 0.1, measured as a 50% solution of lignosulfonate. It should be noted that the preferred pH value is lower than that suggested in Canadian patent 743,861 mentioned at the outset, where a pH value of 3 is mentioned.

The pH of lignosulfonate can also be lowered by other means than by adding acid, for example by Electrodialysis or by ion exchange. The lowering of the pH of lignosulfonate according to the invention increases the curing speed and thereby reduces the

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Pressing times. The invention makes the autoclave! Canadian patent 743 861 mentioned at the outset unnecessary. '·

The pH of a product according to the invention can be increased after pressing by a neutralization treatment will.

The pressing time can be increased by post-curing a partially cured Product "is reduced at elevated temperatures. No increased pressure is required for post-curing, as required in the autoclaving step of the aforementioned Canadian patent 743,861.

Preferred embodiments are described below:

Sulphite waste liquor is z. Z, mostly available either as a solution with f? O ^c / o solids content or as a powder. Therefore, these are the preferred forms for formulating the binder, but the invention is not limited to these forms alone. To make particle board, a 10% solids liquid can be combined with the wood particles, but the mixture should be dried to reduce the moisture content to 6 to 12% of the sheet weight prior to hot pressing. A concentrate of the waste liquor is therefore preferably used.

For the production of the chipboard, the amount of mineral acid to be used for the binder and / or the Press time depending on many factors and their relationships. These factors are discussed below.

a) The acidity of the sulphite liquor used

Calcium, magnesium, and ammonium lignosulfonates are usually more acidic than Uatrium Lignosulfonate.

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More acid is needed, though, to get restorative bonding Sodium lignosulfonate is used.

b) Desired quality of the bond

Generally there are two types of particle board depending on the type of resin mandrel used. The "waterproof" plate is made with phenolic resins, and the "water-resistant" panel with urea resin. The former can be subject to full weathering for outdoor use, resist and will not disintegrate when subjected to the boiling test. the the latter cannot withstand prolonged full weathering and is restricted to indoor use completely disintegrates when subjected to the boiling test. To have a plate of a quality for outdoor use requires more acid or a lower pH.

c) The desired level of pH in the finished plate.

The pH value in the finished plate is mainly determined by the amount of acid in the waste liquor and, secondarily, by the quantity of the modified waste liquor in the plate. High press temperatures and longer pressing times increase the pH of the finished board. If there is a lower pH in the! Finished product is acceptable, a composition can be used which has a high acid content. It should be noted that the plate can be neutralized after pressing, as described below will.

d) pressing conditions

The pressing temperature and time are important factors in the Chipboard manufacture. High temperature requires normal

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wise a short pressing time and vice versa. Waste liquor, the x ^ less Contains acid, requires higher pressing temperatures to produce a product with exterior quality (for outdoor use) and sufficient To achieve curing. Alternatively, the same quality can be achieved by using a long pressing time at lower pressures Press temperatures are generated.

e) Post-curing treatment

The purpose of an IT hardening treatment is to increase the Binding quality and the dimensional stability of the plate. the Post-curing is an important stage in the manufacture of panels with waste caustic, especially when the press temperatures are not high possible are. In general, proper post-curing treatment of a panel can be a "waterproof bond." even if they are insufficiently cured either because of a low acid content or insufficient pressing temperature and time was.

f) Types of wood and shape of the particles

High acidity wood may require modified, less acidic waste liquor. Large particles or thick chips or slices of dense wood tolerate sulphite waste liquor, which contains more acid, better.

g) Fire retardant plates

Phosphoric acid is a very effective fire retardant, however more expensive than sulfuric acid. If the sulphite waste liquor is modified with phosphoric acid as a binder for chipboard, it results this is a fire retardant plate. The amount of phosphoric acid to be added to the waste liquor is generally determined by the degree of fire retardancy desired in the final panel. Usually a much higher salary

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of phosphoric acid than sulfuric acid is required in the waste liquor, for both satisfactory binding and firing delay to reach the plate.

h) Hot press treatment for perfect binders

The effectiveness of the invention can be improved by the lignosulfonate is heated, preferably under pressure, before or after the addition of the acid. It seems that this Heat treatment partially polymerizes the lignosulfonate and, as a result, the pressing time and / or the time needed to achieve a acid required for satisfactory binding.

From the standpoint of production efficiency, it can be summarized that the sulphite waste liquor should be modified with a maximum content of acid in order to achieve the shortest pressing time and yet to obtain the desired quality in the end product. It is true that short press times increase productivity and thus lower costs. However, it should be pointed out that a high content of acid in the sulphite waste liquor can also have certain undesirable effects in the finished board. Acid is detrimental to the strength of the wood as a result of its hydrolysis. The hydrolysis of wood in the presence of strong acid, especially when hot pressing at high temperature, proceeds at a fairly rapid rate. Charring, burns, or even explosions can occur during hot pressing on panels. He &> Igen that are treated with sulphite waste liquor, which has a high acid content. In general, the board with the higher acid content is inferior in strength properties, but more dimensionally stable than a board containing less acid. In addition, a high acid content in the modified sulphite waste liquor leads to low pH values in the finished panel product. High acidity in a board can have a long-term destructive effect on the wood in the board. Additionally can

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Corrosion "occurs in nails and other hardware items that can be used to manufacture products from the plate. Because of this, certain consumers ask for one Minimum pH of around 3 for chipboard. -Im lalle der Manufacture of fire retardant chipboard with phosphoric acid modified The resulting plate generally has a high fire retardancy, but low pH values.

It may be necessary to use post-treatment to reduce the acidity of the low pH plates. This can by neutralizing the acid with ammonia gas, liquid or solution according to known procedures. These Tray treatment with ammonia is able to reduce the acidity of the plate to any desired level without changing the reduce other properties.

Although the above is specific to manufacture of chipboard, which is cited as an example and has been studied most in detail, it was also found that the binder composition is also suitable for other lignocellulose products, xvie bagasse and rice husks or husks. It is also suitable for binding Plywood for making plywood.

A satisfactory adhesive composition can be achieved with lignosulfonate, which has a pH in the range of 2 to 0.1, measured on the basis of a 50% solution of lignosulfonate, which is about 2 to 20 % concentrated sulfuric acid, measured on the Based on weight of lignosulfonate solids, is equivalent. Exterior grade particle board is available at reasonable press times at a pH of about 1.5 "to 0.2, which is equivalent to 3 to 16 % acid based on lignosulfonate solids weight. The higher pHs in this

409837 / 0889-

Area are lighter with a "treated by hot pressing" Binder composition achievable,

For fire retardant particle board, the phosphoric acid content can vary from .20 to 100%, but is preferably in the range of about 30 "to 50 %. Other acids such as hydrochloric acid can also be used, but it is expensive and therefore below current Circumstances not practical.

As already mentioned, both the uachhardening and the hot press treatment the acid requirements and / or the Pressing times.

The modulus of rupture (MOR) increases with increasing proportions of sulphite waste liquor solids. TTm acceptable chipboard to obtain _s are at least 2% Sulfitablaugefeststoffe, "based on the weight of the wood particles, is required.

TJM to obtain acceptable pressing times for production, pressing temperatures of 150 ⁰ C (300 ⁰ F) or consider more than necessary. "

The following examples show details of the invention. It should be noted that some examples refer to Horm CSA-0188 (68) ", the Canadian standard for particle board, which uses the above-mentioned test for internal bond strength (tensile strength perpendicular to the plane of the board in psi) as a measure of the bond quality between The torsion-linear ratio was also used instead, which has proven to be more reliable and much simpler, and found that the torsion-linear ratio expressed in inches-lb (cm-kg) in is approximately equivalent to the respective Anglo-Saxon systems of measurement of the internal bond strength, expressed in psi _3.

example 1

A binder was produced in which 5 parts by weight of concentrated sulfuric acid (technical quality) were thoroughly mixed into 100 parts by weight of ammonium-based sulphite waste liquor with 50% pesticides. The modified liquid

311 ί *

Wheat pine was sprayed onto 100 parts of dry wood in proportions of 25 parts pesticides of the modified liquid. Six homogeneous plates (15 x 15 x 1/2 inches = 58.1 χ χ 38.1 1.27 cm) disk was prepared at temperatures of 204 ⁰ C (400 ⁰ P) at various compression times. Because of the high moisture content (30 %) in the mat or web, two fine sieves were placed on the mat surfaces during the hot pressing. This made it easier for moisture to escape and also avoided the tendency of the panels to stick to flat intermediate panels. The sulfite eye panels were found to be moderately resistant to flammability, a property that conventional panels lack when bonded with urea and phenolic resins. All of these panels (with the exception of Mr. 1) meet the requirements of the CSA 0188 (68) standard for type II (building panels for indoor purposes) types F and G. Detailed details on the manufacturing conditions and properties of the panels are given in the table below compiled.

409837 / 08S9

'. '. Press
No. Temp. Time
Oq (min)
( ⁰ I) density
g / cm ^
(pcf) Torsion-
Shear
(in - Ib:
dry ) _Λ
wet Modulus of rupture
(MOg)
kg / cm
(psi) m (25-foot) Dickenaus
strain water
absorp
tion 2
(Plammaus-
spread) An ISI 1
_ ^
VM
I. 1 204 6
(400) 0.71
(44.2) 40.5 J> - - - - 3 exist (I ¹ SI ' 2 204 8
(400) 0.73
(45.6) 85.5 11.6 102
(1450) 45.6 107.3 '70 in the state laboratory 3 204 10
(400) 0.74
(46.2) 127.2 30.4 112.5
(1600) 40.6 101.2 60 4 204 12
(400) 0.73
(45.7) 125.5 36.5 99
(1410) 37.9 105.0 63 K) 5 204 14
(400) ■ 0.79
(49.1) 129.7 62.9 105.5
(I5OO) 39.0 87.1 65 6 204 16
(400) 0.72
(44.9) 141.1 54.3 - 105.5
(I5OO) 51.8 82.0 70 CD Requirement for CSA 0188 (68) for the CD Chipboard types 3? and G 91.4
(1300) The samples were in water of 70 4 - 2 ⁰ I. (21 _± 1.5 ° C) immersed for 24 hours and tested wet. ρ
The Ilamm Spread Index FSI is based on a 60 cm of 70 in a 60 cm tunnel test should be the test ι (2 foot) tunnel test. 150 or less ^ by class >, related Tunnel test 1 to a 7.6

torium of Canada. The FSI value of commercially available, Chipboard made in Canada is n.oreally over I50 in the 6.3 m tunnel test.

Stripping took place during the soaking.

Example 2

A binder made by thoroughly mixing 50 parts by weight of concentrated phosphoric acid with 100 parts of sodium-based sulfite waste liquor (50 % solids) was sprayed onto milled poplar particles to make three-layer fire retardant particle board. The modified liquid content for the particles of the surface layers (-1 / 64 × mesh) was 20 parts by weight, and for the particles of the core layer (1/8 to 1/4 × mesh) was 15 parts by weight, each of the contaminants of the modified liquid. The ratio of surface material / core material for 12.7 inch thick three-layer panels was 1: 3 »based on weight. Four panels (I5 2 15 1/2 χ = χ 38.1 38.1 χ 1.27 cm) wurdenbei a plate temperature of 204 ⁰ G (400 ⁰ F) and a pressing time of 10 or 12 Iünuten prepared "ying the With phosphoric acid in the modified liquid, the plates obtained were highly resistant to surface flammability. The test results are summarized in the table below.

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No. Press
Temp. Time
(min)
⁰ C 10 density
g / cm
(pcf) Torsion-shear
(in. - Ib.)
dry wet 12th I ¹ SI ² 1 204
(400) 10 0.63
(39.2), 64 12th 37.1 2 204
(400) 10 0.64
(40.0) 70 26th 33.4- 3 204
(400) 10 0.64
(40.3) 62 29 33.8 4th 204
(400) 0.68
(42.2) 74- 33.4-

The samples were boiled and wet in water for 2 hours checked.

The I-lamb spread index S ¹ SI was based on the 60 cm tunnel test. An ISI of 30-40 for a 60 cm tunnel should correspond to a pass of the test on Hasse 2 (5 ¹ SI 75 or lower), based on a 6.3 m tunnel test in the state laboratory of Canada.

Example 3

A binder was prepared by thoroughly mixing 9 parts by weight of concentrated sulfuric acid with 100 parts of magnesium-based sulphite liquor (50 % solids). The modified liquid was sprayed onto poplar chips (0.035 x 1.5 x 1/8 - 2 inches = 0.9 38 χ 3.2 - 51 mm) at the rate of 10 parts of the modified liquid solids per 100 parts of dry wood. The chips treated with liquid contained-

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th about 15 "to 18% moisture content and therefore two fine screens were placed on the surfaces of the mats during hot pressing. Animal chipboard 38.1 38.1 χ χ 1.27 cm were measured at a plate temperature of 204- ⁰ C with pressing times which ranged from 6 to 12 minutes produced. the hot pressed plates were immediately placed in a 177 ⁰ C (350 ⁰ F) heated oven for half an hour Hachhärtungsbehandlung. This post-curing treatment was necessary to improve the bond quality when the hot-pressing time short was. ITachhärtungstemperaturen of 121 ⁰ C and 149 ° C (250 and 300 ⁰ P) were less effective than 177 ° C (35Ο ⁰ P). the test results showed that a Fachhärtung of 2 hours at ⁰ C for about 14-9, the same result provided as an hour at 177 ⁰ C. the prolongation of the Eachhärtungsbehandlung at 177 ⁰ C, the dimensional stability of the plates would greatly improve, but reduce their Pestigkeitseigenschaften. the test results are summarized in the following table:

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Press. '". ■

No. Temp. Time Density in Torsions- Dickenaus- Wasserabsorp

0.66
(41.5) 41, 8th 15, ⁵ 163 111
(2320) (1580) 27.7 0.68
(42.6) 108 8th 44, 5 154.6 101
(2200) (1440)
168.7 123
(2400) (1750) 23.0 0.64
(40.3)
0.69
(4-3.4) 104, 2 50,
56, 6th
9 18.7
22.0

(psi)

• 204 6 0.66 41.8 15.5 - - 27.7 81.2

(400)

204 8 0.68 108.8 44.5 163 111 23.0 77.6

■ o

tT 3 204 10 0.64 91.6 50.6 154.6 101 18.7 '83.2

S 4 204 12 π. μ 104.2 56.9 ^ 68.7 ^ 12 ^ ²² '° ⁷³ » ⁷ ^

-J (400)

^ Requirements according to the standard

<° CSA 0188 (68) for panels type P 40 ⁵ - 140.6 70.3

ITVjU (\ J , ^ - - ■ »- '

(2000) (1000) -J

, cn

The samples were boiled in water for 2 hours and then tested wet.

The samples were boiled in water for 2 hours and tested wet. The Naß M.O.E. (Modulus of rupture) xv was calculated on the dry thickness of the samples before boiling.

^ CSA 0I88 (68) requires an internal bond strength of 2.8 kg / cm = 40 psi, which is about 40 in.-Ib. in the torsion-shear test. .

Example 4-

Commercially available calcium lignosulfonate powder obtained by spray-drying waste liquor was used in this example. 100 parts of poplar shavings were first sprayed with 0.7 parts of concentrated sulfuric acid (diluted in three parts of water) and then mixed with 4 parts of potassium lignosulfonate powder. Three plates of 38.1 38.1 χ χ 1.27 cm (15 15 χ χ 1/2 inch) were pressed at 204- ⁰ C and pressing time 6 to minutes. The hot-pressed panels were immediately placed in an oven heated to 177 ° C for a one hour post cure treatment. The test results are summarized in the following table:

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Press-No. Temperature time density torsion-shear M.O.E. Dickenaus water drainage

⁰ C (min) g / cnr dry wet dry wet elongation sorption ISI

^/ kg / cm τ »τ« ■

1 204 6 0.64 55.4 24.9 154.7 84.4 23.5 (400) (40.0) (2000) (1200)

2 204 ■ 8 0.71 76.2 39.3 168.7 109 23.6 (400) (44.2) (2400) (1550)

3 204 10 0.64 84.8 41.5 143.4 88 90.6

'* - (400) (40.3) (2040) (1250)

tj CSA 0188 (68) requirements'

"^; for plates of type P 40 140.6 70.3 - - so

S. , (2000) (1000) ι

CO. ■■ ι. »■ ■ - —— ·" ■ '"■■' ■ · ~ ———— ⁱ '■■■■

89 , 9 96 80 , 6 95 90 99

Samples were boiled in water for two hours and tested wet.

Samples were boiled in water for two hours and tested wet. The wet M.O.E.

calculated on the dry thickness of the samples before cooking.

- 20 example j?

In this example, poplar chips obtained from a Canadian particle board manufacturer were used. These chips were cut tangentially from round wood by means of a chipper so that they had pointed ends. They were dried to a moisture content of 4 to 5 %. The nominal thickness of the chips was 0.76 mm (0.030 inches) with a controlled length along the pas of 58.1 mm (1 1/2 inches) and with regular widths of 3.2 to 76 mm (1/8 to 3 inches) .

100 parts dry weight of these chips were first sprayed with 0.9 parts of concentrated sulfuric acid diluted with 3 parts of water. The treated chips were then mixed with 5 parts of powdered calcium lignosulfonate (spray-dried sulfite waste liquor). 5 plates 9.5 mm (3/8 ") thick and 38.1 38.1 (15 15") in size were ^{pressed at a plate temperature of 210 °} C (410 ^° J ¹ ) for 4 or 5 minutes. During the hot pressing, Teflon-coated intermediate plates were used to prevent the plates from sticking to the intermediate plates. After pressing (there was no ITachhärtungsbehandlung applied), the plates at 21.1 ⁰ C were conditioned (70 ⁰ F) and 65% relative humidity for two weeks before they were tested. The test results are summarized below.

409837/0869

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409837/0869

Example 6

100 parts (dry weight) of commercially available cardboard chips were first sprayed with 0.6 parts of concentrated sulfuric acid diluted with 3 parts of water. These chips were then mixed with 4 parts powdered calcium lignosulfonate. 5 plates of 38.1 χ 38.1 cm in size and 9 »5 mm (3/8 inch), 12.7 mm (1/2 inch) and 19 mm (3/4 inch) thick were" at plate temperatures of 210 ⁰ C (410 ⁰ I ¹ ) different time periods pressed.

In order to prevent the steel intermediate plates from sticking, first sprayed them with a very thin layer of an oil emulsion, before the mat was formed on the panels. The oil emulsion was mixed with 100 parts by weight of soybean oil (or Mineral oil) and 15 parts of sodium hydroxide (the amount of sodium hydroxide in the oil emulsion was varied depending on the amount of sulfuric acid that was sprayed on the chips). During the hot pressing, the acid vrarde on the particles, the exposed on the surfaces of the mats, neutralized by the sodium hydroxide in the emulsion, which were on the press plates was sprayed on. This neutralization not only prevented the plates from sticking to the press plates, but also reduced it also the darkening of the plate surface. Moreover, this formed on the plate surfaces hardened by the hot press any remaining oil left a protective film on the surface of the plate, which was very water-repellent.

After hot pressing, the panels at 21, 1 ⁰ C and 65% relative humidity were conditioned for two weeks before they were tested. The test results are summarized in the following table.

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Plate thickness Press Time density Torsion-shear wet ² M. 0. E. wet I. mm
(Customs) temperature (min) g / cm ³
(pcf) dry 20.1 kg / cm (psi)
dry ■ 73.8
(1050) 'ro ⁰ C
( ⁰ F) 4th 0.61
'(38.3) 76.4 36.8 156.8
(2230) 102.6
(1460) I. ; 210
(410) 5 0.66
(41.5) 98.6 27.8 244.7
■ (3480) 80.8
(1150) 6th 0.63
(39.1) 93.8 33.8 173 _N.
(2460) 12.7.
(1/2) 10 0.71
(44.5) 100.6 21.8 19th
(3/4) 210
(410) 15th 0.66
(41.4) 68.3 O
CD 210
(410) 837- / 086 "

On samples 2.54 cm (1 inch) square.

The samples were boiled in water for 2 hours and then tested wet.

Example 7

This example shows the hot pressing of sulphite waste liquor bonded plates at a relatively low press plate temperature of 177 C (350 F).

100 parts dry weight of soft maple wood chips (-8 + 10mesh = <2.4 -> 2 mm) were sprayed with a modified sulphite waste liquor. This liquid consisted of 10 parts by weight of powdered calcium lignosulfonate, one part of concentrated sulfuric acid and 4 1/2 parts of water. The wood shavings had a moisture content of about 14% after the binder was applied. 3 mats (38.1 38.1 cm) were formed and prepressed under a pressure of 28 at (400 psi) for 2 minutes. The pre-pressed mats were very compact due to the high tackiness of the modified sulphite waste liquor and could therefore be handled without the use of intermediate plates. All three mats were pressed into sheets of 9.525 mm (3/8 inch) thick plate at a temperature of 177 ⁰ C (35O ° F) for 15,12 and 10 minutes.

However, the mat was sandwiched between two fine screens (40 mesh = 0.42 mm) made of stainless steel during hot pressing. This eliminated sticking and further facilitated the entry of steam from the mat. Immediately after Hot pressing, all panels received a shelf hardening treatment (heating the panels in an oven at one temperature of 149 ° C (300 ° F) for one hour). The test results for these three 9.5 mm panels are as follows Table shown.

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Press

Platt θ-Νγ.

temperature

⁰ C ( ⁰ F)

Time (min)

Density g / cnK (pcf)

Torsion-shear (in-lb)

dry

wet'

M. 0. E.

kg / cm ² (psi)
dry wet

1 177.
(350) - 15th 0.90
(56.5) 185 89 205.3
(2920) 88.6 '
• (1260) 2 177
(350) 12th 0.82.
(51.5) 120 52 170
(2420) 99.8
(1420) 3 177
(350) 10 0.80
(50.0) 110 38 173 ''
(2460) 77.3,
(1100)

O IO OO U)

° On a sample of 2.54 cm square oo

<° The samples were boiled in water for 2 hours and tested wet.

Example 8

This example shows the possibility of producing chipboard with modified waste liquor, the extremely high or has extremely low acid levels. Four modified spent liquors were made for this purpose. The recipes A, "B and C were each with 100 parts by weight of a waste liquor with 50% solids content (calcium lignosulfonate) and 1 or 2 or 3 parts concentrated sulfuric acid produced. Formulation D was made with 100 parts by weight of powdered sodium lignosulfonate and 100 parts of concentrated sulfuric acid diluted with 100 parts of water. Iodine this modified Leaching was carried out on white pine particles (1/4 - 1/8 mesh size) in an amount of 10 parts dry weight sprayed onto 100 parts of white pine particles. The treated particles were formed into a mat (38, 1 χ 38 x1 cm) and by hot pressing into a 7 * 937 ^ (5/16 inch) thick plate that had a density of about 0.64 - g / cm (50 lb), There were a total of 19 plates with the 4 different degrees of acidity made in the Abiaugenbinder. The test results are summarized in the following table. When evaluating this Results, it can be seen from the practical point of view that acid levels outside the range of this example do not have any supply suitable binders for the production of chipboard.

409837/0889

Pr e s s "conditions ~

Plate no. Resin type

O CO 00 Approx

O 00

σ>

(O

1 2

3 4

5 6

7 8

9 10

11 12

13 14

17 *

18 * 19 *

temperature Time Torsion-shear wet M. 0. R. wet (450) ⁰ O (min) (in-lb) _o ' -5 5 (400) ( ⁰ P) dry -5 • kg / cm (psi) ο 5 (350) 210 (410) 120 102 -5. dry 5 (280) 210 (410) 60 98 -5 232 (3300) 5 210 (410) . 12th 97 5 206 (2930) 5 (590) 210 (410) 8th 104 219 (3120) 5 (530) 210 (410) 120 115 - ^5th 200 (2850) 5 (360) 210 (410) 60 130 249 (3540) 5 (670) 210 (410) 40 ^ 28 204 (2900) 5 210 (410) 20th 132 8th 187 "(2660) 31.6 210 (410) 10 80 9 193 (2750) 28 210 (410) 120 54 9 244 (3470) 24.6 210 (410) 60 79 6th 176 (2500) 20th 210 (410) 30th 105 "5 157.5 (2240) 5 210 (410) 20th 77 40 183 (2600) 41.5 210 (410) 10 121 30th .155 (2200) 37.3 121 (250) 60 106 30th 21.1 (300) 25.3 121 (250) 40 107 45 95 (1350) 47 121 (250) 30th 114 3 93 (1320) 149 (300) 10 105 91 ^ 1300) 177 (350) 5 3 104 (1480) 3

ro -ο

CD CD

Comments on the footnotes;

On test specimens 2.54 cm square

ρ
The samples were boiled in water for 2 hours and wet

checked.

^ The mat exploded during hot pressing because of the gas formed by the high acid content.

The finished plates number 15 ^ is 19 were strongly acidic (pH values were around 2).

- ⁷ The stripping took place.

Example 9

The pressing time in minutes required to produce a boil-proof bond in chipboard 9.5 mm (3/8 inch) thick.

/1

keep that with 5% calcium lignosulfonate with various Sulfuric acid contents are bound.

ρ Plate sulfuric acid content in calcium lignofulfonate

temp. ⁰ C 7.5% 10% 12.5% 15% 17.5% 20% 22.5% '100%

204
(400) 20 ^ 10 8 7 6 5 4

177
(350) 40 25 16 12 9 7 6 5

149
(300) 80 50 40 30 25 20 15 10

121
(250) _______ 20

Calcium lignosulfonate solids based on the dry weight of the finished panel "
2 / based on

Weight percent t / calcium lignosulfonate solids

^ the pressing time 'can be shortened by about 20% if after the hot pressing is followed by a post-curing treatment Mat exploded while eating

^ Mat showed signs of charring.

409837/0869

Example 10

pH value of the finished plate (boil-proof bond), which is 5% Calcium lignosulfonate and various sulfuric acid contents

1 is bound

Acidity% 7.5 10 12.5 15 17.5 20 22.5 100

pH of the

Plate 4.1 3.7 3.5 3.3 3.1 2.9 2.6 1.0

. based on

Weight percent / calcium lignosulfonate solids.

Example 11

This example shows chipboard that is bound with sulphite waste liquor, which was cleaned after the addition of acid.

100 parts by weight of commercially available waste liquor (calcium lignosulfonate) at 50% solids became more concentrated, first at 8 parts Mixed sulfuric acid. The acidified eye was then filtered to remove insoluble material, which had precipitated after the addition of acid. The purified binder was in an amount of 5 parts (solid weight) commercial poplar chips were sprayed on 100 parts, and the sprayed chips were used as a core mass for the production of 3 layers of chipboard used.

Another 100 parts of waste liquor were first concentrated with 6 parts Sulfuric acid mixed and then used for removal

409837/0869

cleaned of the precipitate. The cleaned binder was in sprayed an amount of 6 parts dry weight (after cleaning) on 100 parts poplar shavings. The sprayed chips were as a top layer material for the production of 3-layer chipboard used. The ratio between outer layers and core layer was 4: 5, based on the weight of the sprayed Shavings. The test results on four chipboards that were bound with the cleaned resin binder from the sulphite waste liquor are summarized below.

409837 / Q869

Plate no,

Press

TemperatUro _C

( ⁰ F)

Time min

density

g / cnr

(pcf)

Torsion-shear

in-Ib dry wet

M. O. E.

ρ kg / cm (psi)

dry

wet

210
(410) 4th 0.70
(43.8) 110.0 16.3 240
(3410) 79.5 _N
(1130) 2 210
(410) 5 0.67 _N
(41.9) 122.0 26.9 242
(3440) 115
(1630) 3 210
(410) 5 (47.6) 100.5 38.0 261.5
(3720) 122.3 _s
(1740) 4th 210
(410) 6th 0.74
(46.0) 100.5 40.4 256 "
• (3640) 121.6
(1730)

Example 12

This example shows how to work to reduce the

the acidity of the finished chipboard, with the acid-modified

adorned waste liquor are bound. This procedure includes the treatment of the finished panel in a closed container, which is filled with ammonia gas (NH.,) · The duration of exposure mainly depends on the original pH value of the finished panel, the desired degree of neutralization and the panel thickness. This aftertreatment with ammonia can reduce the acidity of the plate to any desired level with no other properties to change. The following table shows the result of this Treatment.

409837/0889

HOW DOES DEE AMMONIA NEWTEALIZATION EFFECT ON PLATE ACIDITY AND TORSION FASTENING STRENGTH?

Plate- thickness Exposure time pH before after OJorsion 'shear before after No. mm
(Customs) Min. in-rb 80.7 89.4 9.5 (3/8) 2.76 6.73 48.1 53.1 1 9.5 (3/8) 30th 2.92 7.25 69.1 72.0 2 9.5 (3/8) 30th 2.89 6.65 · 102.7 97.9 3 9.5 (3/8) 20th 2.82 5.56 120.9 120.3 4th 9.5 (3/8) 20th 2.78 4.76 99.5 103.4 5 12.7 (i / 2) 10 2.80 6.15 92.6 91.6 6th 12.7 (1/2) 30th 2.63 • 4.91 115.1 121.4 7th 12.7 (1/2) 20th 2.79 3.70 83.2 80.9 8th 19.0 (3/4) 10 2.80 3.98 121.2 109.7 9 19.0 (3/4) 30th 2.59 4.12 10 30th

Example 13

This example shows the possibility of removing calcium ions without adding acid to the waste liquor · Calcium-based waste liquor (50 % solids) was first diluted to 25% solids · with water and then passed through a column of cation exchange resin {BEXYN 101, an organic, strongly acidic cation exchanger ). The calcium ions in the waste liquor were removed by the cation exchange resin. The demineralized waste liquor after concentration to 50 % solids content shows a pH value of less than 1 and behaved like a waste liquor modified with acid. *

The demineralized waste liquor was sprayed onto hammer milled white pine particles (1/8 - 1/4 inch = 3.17 - 6.35 mm) in the amount of eight parts of demineralized liquor solids on parts of dry wood. The resin-coated particles were at 77 ⁰ C (170 ⁰ F) for about 10 minutes in the oven-dried to reduce the moisture content to about 5 - 6% decrease before the mat has been formed. 4 homogeneous plates (38.1 χ χ 38.1 9.5 MRO) were produced at a sheet temperature of 210 ⁰ C at a pressure of 42 kg / cm (600 psi). Two intermediate plates coated with Teflon were placed on the mat surfaces during hot pressing. The test results are summarized below.

409837/0889

Plate-irr,

. Press temperature time

⁰ C min

( ⁰ F)

Dense torsional shear

g / cm * in-lb

Cpcf) dry wet

• MOE kg / cm ² (psi) dry wet

210 (410)

0.68 (42.7)

130

12th

102 (1450)

60, <(860 '

210 (410)

210 (410)

210 (410)

0.72 _n (45.3)

0.77 _N (48.2)

0.80 (49.7)

142

158

173

24

32

43.

129 (18 ^ 0)

157 (2230)

167 (2370)

77.0 (1100)

85 (1210)

90 (1280)

Example 14

This example shows the possibility of manufacturing particle board bound with acidified calcium lignosulfonate powder. The acidified powder was first prepared by mixing certain amount of sulfuric acid with 50% waste liquor, and the mixture was then at a temperature of 149 ⁰ C (30O ⁰ F) sprühgetrock net. Two powdered binders with two acid contents for the production of particle board were produced. The powder ■ with the higher acid content, which contained 7 parts by weight of concentrated sulfuric acid to 100 parts by weight of calcium waste liquor with 50% solids content before spray drying, was used as a binder for the core layer of particle board. The lower acid powder, which had 6 parts by weight of concentrated sulfuric acid to 100 parts by weight of 15% solids calcium waste before spray drying, was used as a binder for the top layers of the panel. The acidified powder was mixed with poplar chips in an amount of 4 parts by weight per 100 parts of dry chips. After mixing, the fine powder (100 mesh = 0.15 mm) adhered well to the chip surfaces. The ratio of top side / core / top side material for chipboard with a thickness of 9.5 mm was 1: 2: 1 parts by weight. 6 Poplar wood (38.1 38.1 χ χ 9j5 mm) were prepared at a plate temperature of 210 ⁰ C and a pressure of 28 atmospheres (400 psi). The test results are shown below.

409837/0869 ORfQiNAL. inspected

■ Platte-Hr. Press Time density Torsion-shear • M. O. E. (psi) temperature Min g / cm * in-lb wet kg / cm wet ⁰ C (pcf) dry 18th dry . 75 1.2 C op) 4th 0.64 99 207 (1070) 210 (40.1) ⁺ 22nd (2940) 92 3.4 (410) 5 0.66 99 221 (1310) 210 (41.4) 25th (3140) 84 * ·> 5.6 (410) 6th 0.63 82 197 (1200) (O
OO 210 (39.1) , (2800) approx (410) / 0869

* Each number shows the average value of 2 plates «

Example 15

This example shows the possibility of using the modified waste liquor as a binder for chipboard made with materials other than wood. A binder was prepared by thoroughly mixing 8 parts by weight of concentrated sulfuric acid with 100 parts of calcium-based aqueous solution containing 50% pesticides. The modified liquid was applied to each of bagasse splinter (1/8 - 1/4 mesh) and white pine bark particles (1/8 - 1/4 mesh) in an amount of 8 parts of modified waste solids to 100 parts of dry bagasse t> zw. Sprayed on bark. The liquid coated splinters and particles were dried in an oven at a temperature of 77 ° C (170 ° F) to achieve a moisture content of about 5 to 6% before the mat was formed and hot pressed. 6 plates (38.1 χ 38.1 χ 0.95 cm, namely 3 plates each from bagasse and from bark) were at plate ^{temperatures of 200 0} C (400 ⁰ F) at a pressure of 28 to 42.2 kg / cm ² (400 to 600 psi). The test results are summarized below.

409837/0869

Table 18

Plate- temp. Press Time No. ⁰ C (min)

density

g / cnr Cpcf) torsional shear
(in-lb)

dry

wet

kg / cm (psi) dry wet

Bagasse

O
(O
OO

1
2

204
(400)

204
(400)

5
5

0.72 _s (45.2)

0.81 (50.6)

7/0 3. 204
(400) 5 0.89 _n
(55.3) 869 bark 4th 204
(400) • 5 0.88
(54.9) 5 204
(400) 6th 0.89
(55.7) 6th 204
(400) 7th o, 90
(56.1)

21
29
33

19th
24
26th

108 (1540)

164.5 (2340)

179 _n (2530)

44 (620)

(750)

49 (700)

28 (400)

45 (640)

56 (800)

8 (110)

12th

(170), S ₀

16 Ξ (230) ο

CJ)

Example 16

This example shows the possibility of using the modified waste liquor as an adhesive binder for plywood. The sulfite waste liquor (calcium base, 50% solids) was first mixed thoroughly with 5 parts by weight of concentrated sulfuric acid to 100 parts by weight of the 50% solids waste liquor and then filtered to remove the calcium precipitates. Douglas pine and poplar boards (3 »2 mm χ 30.5 x 30.5 cm, 2 - 3% moisture content) were treated with the modified waste liquor in an amount of 261.5 g solids per m (15 g solids per square foot) coated. The veneer boards coated with binder were layered on top of one another, the time it took them 4-5 minutes before hot pressing when the press was closed was 2 sheets of three-layer plywood (each douglas pine and poplar) were 5 minutes at 177 ° C hot pressed at a plate pressure of 10.5 kg / cm ² (150 psi). When the plywood panels were tested under both dry and wet conditions, the cracked surface showed a high percentage of failure in the wood.

Example 17

This example shows the possibility of producing wood-filled moldings with the acidified powder of calcium linosulfonate. The acidified waste liquor powder was obtained by spray drying a mixture consisting of 5 parts by weight of concentrated sulfuric acid and 100 parts by weight of waste liquor (50% solids). The spray-drying temperature was 149 ° C (300 ⁰ F) and the fine powder was

sifted through a 0.15 mm (100 mesh) sieve

20 percent by weight of the powder resin was used thoroughly

409837/0869

with 100 parts dry weight of white pine particles (100 mesh and 5% moisture content). A disc 10.16 cm (4 inches) in diameter and 12.7 mm in thickness was made at a die temperature of 177 ° C at a Pressure of 70.3 kg / cm and a pressing time of 20 minutes. The disc had a specific gravity of 1.1 and showed good strength and dimensional stability.

Example 18

This example shows the possibility of heat treatment for sulphite waste liquor at high temperature in order to reduce the amount of acid required for the perfect binder. About 800 mm of calcium lignosulfonate liquid (50% solids) was first placed in a cylindrical steel vessel of about 1000 ml volume and this was tightly sealed. The sealed vessel was about 2 hours immersed in a heated to a temperature of 177 ⁰ C oil bath. During this heating period, the pressure in the vessel gradually increased to 1913 kg / cm · (275 psi) or more. The heat and pressure treated liquid became darker and more viscous as it partially polymerized.

A binder was prepared by thoroughly mixing 20 parts by weight of a 20% sulfuric acid solution with 100 parts by weight of the treated lignosulfonate liquid (about 50% solids). The modified liquid binder was sprayed onto commercially available poplar chips in an amount of 5 parts by weight of binder liquid solids to 100 parts of dry chips. The binder treated chips were dried for 5 minutes by hot air of 66 ° C (150 ⁰ F) to reduce the moisture content of the chips to be reduced to about 8 to 10%. 3 homogeneous plates (38.1 × 38.1 × 0.95 cm) were produced at a plate ^{temperature of 204 °} C. and a 7-minute pressure of 28.1 kg / cm. 2 intermediate plates coated with Teflon were placed on the mat surfaces during

409837/0869

of hot pressing ^ placed on. The test results are in of the following TabeXe.

0.66
(41.5) lorsion shear M.O.E. » wet 0.68
(42.6) (in.-Ib)
dry . wet kg / cm ^£
, (psi)
dry 79.5 _N
(1130) Plate density,
No. g / enr
(psf) 0.70
(44.0) 92 18 "195.5
(2780) 87
(1240) 1 116 31 204
(2900) 100
(1420) 2 110 27 213.7
(3040) 3

The comparison of the above results with those of Example 14 shows the effectiveness of the treatment which allows lower amounts of acid for comparable results to use.

It was further found that the hot skewer treatment also can be applied to a composition in which the lignosulfonate and the mineral acid have been combined. With the inclusion of the acid, the treatment time becomes considerable reduced, the treatment time depending on the temperature, the pressure and the composition.

Based on the above findings, the presently preferred mode of operation for making a perfect binder includes in dry powder form the stages

1. the combination of concentrated sulphite waste liquor with acid,

2. removal of the precipitate if desired, 3- application of heat and pressure treatment; and 4. spray drying.

409837/0869

In an older proposal (P 24 02 440.6) is a procedure for pressing particle board using steam in a press with a pair of press plates, each Plate has openings in the surface facing the other plate, and wherein the press has a sealing device which defines a chamber which defines the space between the Plates enclosing and wherein a mat or a fleece of wood particles and thermosetting adhesive binder is pressed by pressurized steam, preferably saturated steam, is introduced into and out of the mat through the openings of a press plate the openings of the other press plate, with the steam outlet to maintain an increased pressure and limited to an elevated temperature for a time sufficient to cure the adhesive binder and eventually the steam the sealing chamber drains and separates the press plates for removing the chipboard. It is useful to build up a pressure in the chamber of the steam outlet blocked or restricted until a predetermined pressure is reached in the press. Preferred the direction of flow of the steam can be reversed and the mat can be pre-pressed before the steam is pressed.

The present method is particularly suitable for combination with the steam pressing described above, since it has been found found that pressing with steam injection requires less mineral acid to obtain comparable results to obtain. It is believed that the vapor releases organic acid from the wood particles, making more acid available makes that is necessary for the procedure. So show steam-pressed Chipboard has a lower pH. In addition to the benefit of the lower amount of acid required, there is also damage of wood particles due to hydrolysis, which can cause acid, is negligible. Roughly about 1/4 of the acid is required, which was required in previous processes for the production of pressed chipboard using sulphite waste liquor, to achieve comparable results. Steam pressing can give satisfactory results with an acidity of only

409837/0869

_ / 1 / I _

2%, measured as concentrated suspension "., Acid and related based on the weight of the sulfate solids.

L INSPECTED

409837/0869

Claims (26)

Claims 1. Binder composition for binding lignocellulosic materials, characterized by a concentrate containing lignosulfonate, which is used to achieve a pH value of no more than about 2, measured as a solution of the concentrate at 50% solids. 2. Composition according to claim 1, characterized in that the pH value by means of replacement of cations by hydrogen ions is humiliated. 3. Composition according to claim 2, characterized in that that the pH is lowered by adding a mineral acid. 4-, composition according to claim 2, characterized in, that the pH value is lowered by means of electrodialysis, 5. Composition according to claim 3, characterized in that the mineral acid is sulfuric acid. 6. The composition according to claim 1, characterized in that the solution with 50% solids has a pH between We _r t, having about 0.1 and about. 2 7. Composition according to claim 6, characterized in that the pH is in the range from 0.2 to 1.5. 8. Composition according to claim 1 ,. characterized in that it is in a dry powdered form. 9 · Composition according to claim 3j, characterized in that that the resulting precipitate is removed. 409837/0869 10. Composition according to claim 1, characterized in that that it is heated under pressure to achieve partial polymerization. 11. Method of making an adhesive binder for Lignocellulosic materials made from a concentrate of lignosulphonate, characterized in that 1. the concentrate to achieve a pH value of not more than about 2, measured as a solution of the concentrate with 50% solids, treated and 2. heated the lignosulfonate concentrate for partial polymerization. 12. The method according to claim 11, characterized in that stage 2 is carried out after stage 1 is. . Method according to claim 11, characterized in that that the treated and heated concentrate further to achieve an adhesive binder .in dry powder Form is spray dried. . Process for the production of chipboard, characterized in that a mixture of lignocellulose particles, ligriinsulphonate in a proportion which is at least 2 percent by weight of solids, based on the particle weight equivalent, of a mineral acid in an amount of 2 to 20 percent by weight, measured as concentrated sulfur syrup and on the weight of Ligninsulfonatfeststoffe is equivalent based forms, forms a mat or web of the mixture and the mat (300 ⁰ F) or more in the heat pressed at a temperature of about 150 ⁰ C. 15. The method according to claim 14, characterized in that that first the mineral acid and the lignocellulose particles are mixed and then with lignosulfonate in 409837/0869 . 241Q746 powdered form is mixed. 16. The method according to claim 14, characterized in that the lignosulfonate is used in the form of a liquid and first lignosulfonate and mineral acid are mixed and then spray dried and thereafter mixed with the lignocellulosic particles. 17 · "Method according to claim 16, characterized in that - the liquid mixture of lignosulfonate and mineral acid under pressure up to partial polymerization before the Spray drying is heated. 18. The method according to claim 14, characterized in that the proportion of mineral acid to solid lignosulfonate, in terms of weight, is 4 * "to 16%". 19 · "Method according to claim 14, characterized in that sulfuric acid is used as the mineral acid. 20. The method according to claim 14, characterized in that. to achieve fire retardant plates as mineral acid Phosphoric acid is used. 21. The method according to claim 14, characterized in that the mat for consolidation and partial hardening of the chipboard -hot pressed and the partially hardened Chipboard for sufficient time to harden the chipboard to the desired degree of elevated temperature is subjected. 22. The method according to claim 14, characterized in that the plate after pressing to decrease its acidity 409837/0869 is treated. 23 · The method according to claim 14, characterized in that that first lignosulfonate and acid combined and then removing insoluble material prior to mixing with the lignocellulosic particles. 24. The method according to claim 14, characterized in that that "lignosulphonate is used, which is obtained from sulphite waste liquor is preserved. 25- composition according to claim 1, characterized in, that the lignosulfonate contains calcium, ammonium, magnesium or sodium lignosulfonate. and 25 26. Use of the binder composition according to claims 1 - 10 / when pressing particle board from a mat of wood particles and a thermosetting adhesive binder using Steam in a press with a pair of press plates and means for delimiting a sealing chamber between the press plates, wherein via openings in the facing surfaces of the press plates pressurized steam through the Openings of one press plate are introduced into the mat and drained from the openings of the other press plate and wherein the steam outlet to maintain an elevated pressure and temperature for a hardening of the Adhesive binder is limited in sufficient time and eventually the steam is vented from the sealing chamber and the chipboard is removed from the press. 27- Application of the method according to claims 11-24 for steam pressing of chipboard according to claim 26. 409837/0869