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Patent 2256398 Summary

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(12) Patent Application: (11) CA 2256398
(54) English Title: FIREPROOFING AGENT FOR PARTICLE OR FIBRE BOARDS
(54) French Title: AGENT DE PROTECTION CONTRE LES INCENDIES POUR PANNEAUX EN COPEAUX OU EN FIBRES
Status: Dead
Bibliographic Data
(51) International Patent Classification (IPC):
  • C09K 21/04 (2006.01)
  • A62D 1/00 (2006.01)
  • B27K 3/32 (2006.01)
  • B27N 9/00 (2006.01)
  • C09K 21/02 (2006.01)
  • D21J 1/08 (2006.01)
  • E04C 2/16 (2006.01)
  • E04F 19/02 (2006.01)
(72) Inventors :
  • NOPPER, HERBERT G. (Germany)
  • SCHMIDT, HUBERT F. (Germany)
(73) Owners :
  • NOPPER, HERBERT GEORG (Germany)
(71) Applicants :
  • NOPPER, HERBERT G. (Germany)
  • SCHMIDT, HUBERT F. (Germany)
(74) Agent: SMART & BIGGAR
(74) Associate agent:
(45) Issued:
(86) PCT Filing Date: 1997-05-28
(87) Open to Public Inspection: 1997-12-11
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/EP1997/002780
(87) International Publication Number: WO1997/046635
(85) National Entry: 1998-11-27

(30) Application Priority Data:
Application No. Country/Territory Date
196 21 606.0 Germany 1996-05-30

Abstracts

English Abstract




The invention concerns a fireproofing agent which can be applied to boards or
shaped parts of particles or fibres, obtained from wood or components of
annual plants, in order to render them fireproof. The fireproofing agent
according to the invention contains between 65 and 85, preferably 74, parts by
weight ammonium sulphate, between 10 and 25, preferably 19, parts by weight
borax and between 4 and 10, preferably 7, parts by weight trisodiumphosphate.
In addition, between 0.5 and 2 parts by weight, preferably 1 part by weight,
sodium metasilicate can be added. The invention further concerns a method of
fireproofing boards or shaped parts of this type. According to this method,
the particles or fibres are first impregnated with a solution of the
fireproofing agent according to the invention, are then dried to a moisture
content of between approximately 1 % and approximately 12 %, preferably
between 1 and 4 %, are subsequently glued with a binder, combined to form
pressed mats, and finally compressed to form boards or shaped parts.


French Abstract

L'invention concerne un agent de protection contre les incendies permettant de conférer des propriétés ignifuges à des panneaux ou à des pièces moulées en copeaux ou en fibres, d'origine ligneuse ou provenant de plantes annuelles. Cet agent de protection contre les incendies contient entre 65 et 85, de préférence 74 parties en poids de sulfate d'ammonium, entre 10 et 25, de préférence 19 parties en poids de borax et entre 4 et 10, de préférence 7 parties en poids de phosphate trisodique. Il est possible d'ajouter au mélange entre 0,5 et 2 parties en poids, de préférence 1, de métasilicate sodique. L'invention concerne en outre un procédé permettant de rendre de tels panneaux ou de telles pièces moulées ignifuges. Selon ce procédé, les copeaux ou les fibres sont d'abord imprégnés avec une solution de l'agent de protection contre les incendies proposé, puis sont séchés jusqu'à ce que leur teneur en humidité soit comprise entre approximativement 1 et approximativement 12 %, de préférence entre 1 et 4 %, avant d'être encollés avec un liant, d'être assemblés pour former un non-tissé obtenu par compression, puis pour finir, d'être comprimés pour former des panneaux ou des pièces moulées.

Claims

Note: Claims are shown in the official language in which they were submitted.



-9-
claims

1. Fire-protection agent for sheets or moldings
made from chips or fibers which have been obtained from
timber or from constituents of annual plants, composed
of:
from 65 to 85 parts by weight, preferably 74 parts by
weight, of ammonium sulfate (NH4)2SO4;
from 10 to 25 parts by weight, preferably 19 parts by
weight, of borax Na2B4O7-10 H2O;
from 4 to 10 parts by weight, preferably 7 parts by
weight of trisodium phosphate Na3PO4-12 H2O.
2. Fire-protection agent according to Claim 1,
characterized in that it additionally comprises from
0.5 to 2 parts by weight, preferably 1 part by weight,
of sodium metasilicate, Na2SiO3-9 H2O.
3. Fire-protection agent according to one of
Claims 1 or 2, characterized in that it has been
dissolved in water.
4. Fire-protection agent according to Claim 3,
characterized in that the solution has a concentration
of from 20 to 50%, preferably from 30 to 35%.
5. Board made from chips or fibers which have been
obtained from timber or from constituents of annual
plants, comprising a fire-protection agent with the
following constituents:
from 65 to 85 parts by weight, preferably 74 parts by
weight, of ammonium sulfate, (NH42SO4;
from 10 to 25 parts by weight, preferably 19 parts by
weight, of borax, Na2B4O7-10 H2O;
from 4 to 10 parts by weight, preferably 7 parts by
weight of trisodium phosphate, Na3PO4-12 H2O.
6. Board according to Claim 5, characterized in
that the fire-protection agent additionally comprises
from 0.5 to 2 parts by weight, preferably 1 part by
weight, of sodium metasilicate, Na2SiO3-9 H2O.




-10-
7. Board according to one of Claims 5 and 6,
characterized in that the ratio of the dry weight of
the fire-protection agent to the dry weight of the
chips or fibers is from 0.1 to 0.4, preferably 0.2.
8. Molding made from chips or from fibers which
have been obtained from timber or from constituents of
annual plants, comprising a fire-protection agent with
the following constituents:
from 65 to 85 parts by weight, preferably 74 parts by
weight, of ammonium sulfate, (NH4)2SO4;
from 10 to 25 parts by weight, preferably 19 parts by
weight, of borax, Na2B4O7-10 H2O;
from 4 to 10 parts by weight, preferably 7 parts by
weight of trisodium phosphate, Na3PO4-12 H2O.
9. Molding according to Claim 8, characterized in
that the fire-protection agent additionally comprises
from 0.5 to 2 parts by weight, preferably 1 part by
weight, of sodium metasilicate, Na2SiO3-9 H2O.
10. Molding according to one of Claims 8 or 9,
characterized in that the ratio of the dry weight of
the flame retardant to the dry weight of the chips or
fibers is from 0.1 to 0.4, preferably 0.2.


-10-

11. Process for providing fire resistance to sheets
or moldings made from chips or from fibers which have
been obtained from timber or from constituents of
annual plants, with the following steps:
- the chips or fibers are impregnated with a
fire-protection agent in a solution whose dissolved
constituents are composed of:
from 65 to 85 parts by weight, preferably 74 parts
by weight, of ammonium sulfate (NH4)2SO4;
from 10 to 25 parts by weight, preferably 19 parts
by weight, of borax Na2B4O7-10 H2O;


-11-

from 4 to 10 parts by weight, preferably 7 parts
by weight of trisodium phosphate Na3PO4-12 H2O;
- the impregnated chips or fibers are dried to a
moisture content of from about 1 to about 12%,
preferably from 1 to 4%,
- a glue in the form of a binder is applied to the
impregnated and dried chips or fibers,
- the impregnated and dried chips or fibers, to
which a glue has been applied, are compressed to
give pressed mats and then press-molded to give
sheets or moldings.
12. Process according to Claim 11, characterized in
that the dissolved constituents of the solution of the
fire-protection agent additionally comprise from 0.5 to
2 parts by weight, preferably 1 part by weight, of
sodium metasilicate, Na2SiO3-9 H2O.
13. Process according to one of Claims 11 or 12,
characterized in that the solution of the
fire-protection agent has a concentration in the solution of
from 20 to 50%, preferably from 30 to 35%.
14. Process according to one of Claims 11 to 13,
characterized in the impregnation of the chips or
fibers takes place in a dip bath.
15. Process according to one of Claims 11 to 13,
characterized in that the impregnation of the chips or
fibers takes place in a continuous mixer or in a screw
mixer.
16. Process according to one of Claims 11 to 15,
characterized in that the impregnated chips or fibers
are freed from excess solution of the fire-protection
agent in a dewatering screw device.


-11-
17. Process according to one of Claims 11 to 16,
characterized in that the solution of the
fire-protection agent has a pH in the slightly alkaline
region, preferably around 8.5.


-12-
18. Process according to one of Claims 11 to 17,
characterized in that the impregnated and dried chips
or fibers have a pH of from 3.5 to 4.5.
19. Process according to one of Claims 11 to 18,
characterized in that the binder is composed of urea
resins or of melamine resins.
20. Process according to one of Claims 11 to 18,
characterized in that PMDI resins are used as binders
for chips or fibers made from straw.
21. Process according to one of Claims 11 to 20,
characterized in that the pressed mats are press-molded
at temperatures of from 180 to 220°C and at pressures
of from 150 to 300 N/cm2, to give sheets or moldings.

Description

Note: Descriptions are shown in the official language in which they were submitted.


CA 022~6398 1998-11-27

FiLF.puLl~T~J~
PCT/EP 97/ 02780 i ~ .
P 4818/97-PCT
April 23, 1998

Description

The invention relates to a fire-protection
agent for sheets or moldings made from chips or fibers
which have been obtained from timber or from
constituents of annual plants, and also to such boards
and moldings which comprise a fire-protection agent of
this type. The invention also relates to a process for
providing fire resistance to such sheets or moldings.
Sheets or moldings of the type described are
generally very flammable. However, their material
properties give them a variety of applications as
working materials, for example in furniture
construction and the interior fitting of buildings, and
also in motor vehicles. In many of the possible uses,
however, the ready flammability of the particle boards
or fiberboards and moldings, deriving from the ready
combustibility of the organic raw materials used, is a
disadvantage. Especially in the building industry, it
is desirable on safety grounds to use only working
materials which have low flammability or are fire-
resistant.
Attempts have continually been made in the past
to provide fire retardancy or fire resistance to boards
of timber materials and boards made from sustainable
raw materials. For example, DE 31 44 773 A1 proposes
applying an aqueous solution of inorganic salts to
wood-chip granules which are to be press-molded to give
a wood-chip molding, and then applying glue to the
granules and press-molding these. However, it is also
necessary according to this prior art additionally to
apply a fire-resistant layer to the surfaces of the
wood-chip moldings in order to be able to produce wood-


AMENDED SHEET


.. ..... . ..

CA 02256398 1998-11-27

- la -
chip moldings which are not just fire-retardant but




P~MENDED SHEET



.. ..

CA 022~6398 1998-11-27


A process for providing fire resistance to a
cellulose material has been described in DE 29 23 587
Al. In this it is claimed that the cellulose material
is impregnated with phosphoric acid and with an aqueous
solution which comprises at least one amonium [sic]
salt, for example amonium [sic] sulfate. Other
substances, such as borax and trisodium phosphate, may
be added here. The main constituent of this known
impregnating solution is phosphoric acid, to which the
desired flame-retardant effect is primarily attributed.
An impregnating solution of this type is, however, not
usable when producing particle boards or fiberboards,
since the phosphoric acid gives them an acid reaction
and the binders used when producing particle boards and
fiberboards would precure before the compression
procedure, and this would be extremely disadvantageous.
An example of the provision of flame retardancy
to timber is given in CN 1 100 592. This prior art,
however, likewise does not concern itself with the
provision of fire resistance to particle boards and
fiberboards or to moldings in which the chips and/or
fibers have already been impregnated with a fire-
protection agent during the production process.
The object on which the invention is based is
therefore to propose a fire-protection agent which can
be used to provide fire resistance to sheets or
moldings made from




AMENDED SHEET

CA 022~6398 l998-ll-27

WO 97/46635 - 2~- PCT/EP97/02780

The objcct on ~h;ch thc invcntion ~ ,
therefore to propose a ~ t which can
be used to ~rovid~~~~ire resistance to boards or
~ g~ m~dc -f- ~ chips or fibers which have been
obtained from timber or from constituents of annual
plants. A further object of the invention is to provide
boards and moldings of the type described which are
fire-resistant or highly fire-resistant, and also to
propose a process for providing fire resistance to
boards or moldings of the type described. The fire-
protection agent proposed here must be compatible with
the usual binders for gluing the chips or fibers and
when exposed to a flame must not evolve any smoke gases
hazardous to health.
According to the invention, this object is
achieved by means of a fire-protection agent which
comprises from 65 to 85 parts by weight, preferably 74
parts by weight, of ammonium sulfate, from 10 to 25
parts by weight, preferably 19 parts by weight, of
borax and from 4 to 10 parts by weight, preferably 7
parts by weight, of trisodium phosphate. The moldings
and boards proposed according to the invention comprise
this fire-protection agent.
The process according to the invention for
providing fire resistance to boards or moldings of the
type described at the outset includes the following
steps:
- the chips or fibers are impregnated with the
proposed fire-protection agent in a solution,
- the impregnated chips or fibers are dried to a
moisture content of from about 1 to about 12%,
preferably from 1 to 4%,
- a glue in the form of a binder is applied to the
impregnated and dried chips or fibers,
- the impregnated and dried chips or fibers, to
which a glue has been applied, are compressed to
give pressed mats and then press-molded to give
boards or moldings.

CA 022~6398 1998-11-27

WO 97/46635 - 3 - PCT/EP97/02780

The proposed fire-protection agent is a mixture
of inorganic salts which do not comprise any chlorides
and are nontoxic. It is compatible with all known
condensation resins and polymerization resins, for
example urea resins, melamine resins and phenol-
formaldehyde resins, epoxy resins, novolak resins, PMDI
resins, etc. In addition, it does not give rise to any
volatilization of harmful gases from the finished sheet
or molding.
The ammonium sulfate present in the proposed
fire-protection agent promotes the surface-
carbonization of cellulose via formation of sulfuric
acld .
Borax swells on heating and additionally acts
as a disinfectanti it also serves as an agent for melt
flow during press-molding of the pressed mats. The
trisodium phosphate which is also present in the fire-
protection agent decomposes from 75~C to give NaOH and
P2Os; it has emulsifying, water-softening and buffering
properties.
Mixing these three salts in the ratio given
produces a fire-protection agent which can be used to
provide fire resistance to boards or moldings made from
chips or fibers which have been obtained from wood or
from constituents of annual plants.
An advantageous further development of the
novel fire-protection agent consists in admixing
additionally from 0.5 to 2 parts by weight, preferably
1 part by weight, of sodium metasilicate. Sodium
metasilicate has a water-softening effect and acts as a
wetting agent, and also as a disinfectant, and on
heating releases water. If it is admixed with the fire-
protection agent in a solution it serves as a wetting
agent and thus promotes the wetting of the chips or
fibers with the fire-protection agent. An advantageous
side effect consists in the fungicidal and insecticidal
properties which the fire-protection agent obtains as a
result of admixing of the sodium metasilicate.

CA 022~6398 l998-ll-27

WO 97/46635 - 4 - PCT/EP97/02780

The proposed fire-protection agent is most
advantageously used if it is present in an aqueous
solution, where the concentration of the solution may
be from 20 to 50%, preferably from 30 to 35%. The chips
or fibers may be saturated and thus impregnated with an
aqueous solution of this type before the glue is
applied and before press-molding to give boards or
moldings.
To achieve the other objects the invention
proposes boards or moldings made from chips or fibers
which have been obtained from timber or from
constituents of annual plants and which comprise the
abovementioned novel fire-protection agent. This fire-
protection agent may include ammonium sulfate, borax
and trisodium phosphate in the mixing ratios given
above or, as an advantageous further development,
additionally comprise sodium metasilicate.
The boards or moldings have the best flame-
retardant properties if the ratio of the dry weight of
the proposed fire-protection agent to the dry weight of
the chips or fibers is from 0.1 to 0.4, preferably 0.2.
According to the invention, fire-resistant
boards or moldings made from chips or fibers are
produced using the process described in Claim 11. A
solution of the proposed fire-protection agent is
therefore used to preimpregnate the chips or fibers,
the chips or fibers being saturated with the solution.
The fire-protection agent here may comprise the mixture
of salts given in Claim 1 or the mixture of salts
described in Claim 2. The fire-protection agent is
preferably present in an aqueous solution with a
concentration of from 20 to 50%, preferably from 30 to
35%. The preimpregnation of the chips or fibers with
the fire-protection agent may take place in a dip bath
or else by injecting the fire-protection agent into a
continuous mixer or into a screw mixer. The density of
the solution used of the fire-protection agent is



,,

CA 022~6398 1998-11-27

WO 97/46635 - 5 - PCT/EP97/02780

preferably about 1.2 g/cm3, and its pH is slightly
alkaline, preferably about 8.5.
For the application of glue to the chips or
fibers, their moisture content must not usually exceed
about 12%. It is therefore necessary, after the
impregnation with an aqueous solution of the fire-
protection agent, to dry the impregnated chips or
fibers. After the drying, the impregnated chips or
fibers have a pH of from about 3.5 to 4.5.
Urea resins or melamine resins are preferably
used for the glue application to the chips or fibers
impregnated with the fire-protection agent. A great
advantage of this is that the ammonium sulfate present
in the fire-protection agent dissociates during the
press-molding of the chips or fibers due to the heating
which occurs during that process, and functions as a
curing agent for the binder. This means that it is not
necessary to add a separate substance as a curing
agent. In the case of chips or fibers made of straw,
however, PMDI resins are preferably used as binders.
Using the novel process it is possible to
produce boards or moldings made of chips or fibers,
which are fire-resistant to highly fire-resistant
without the need to apply an additional fire-retardant
coating.
The invention is further explained below using
two examples.

Example 1:
Pine chips were obtained in a known manner by
chipping logs in such a way that their length was from
5 to 15 mm, their width from 2 to 4 mm and their
thickness from 0.2 to 0.5 mm. These chips were predried
to a moisture content of about 30%.
A solution of the fire-protection agent of the
following composition was added to the predried chips
in a continuous mixer:

CA 022S6398 l998-ll-27

WO 97/46635 - 6 - PCT/EP97/02780

50 parts by weight of water,
37 parts by weight of ammonium sulfate,
9.5 parts by weight of borax,
3.5 parts by weight of trisodium phosphate.




The ratio of the weight of the solution added
of the fire-protection agent to the dry weight of the
chips was 0. 6.
The impregnated chip material was then dried in
a drum drier to a residual moisture of about 1% and fed
into a mixer for applying glue. In the mixer for
applying glue, an aqueous binder of the following
composition was added to the impregnated chip material:

82.5 parts by weight of liquid urea-formaldehyde resin
(65% strength),
5 parts by weight of paraffin emulsion (50% strength),
12.5 parts by weight of water.

In this step there was no need to add a
substance as a curing agent, since the dried
impregnated chip material had a pH of from 3.5 to 4 and
the fire-protection agent added therefore functioned as
a curing agent on compression. The ratio of the weight
25 of the aqueous binder to the weight of the dried,
impregnated chip material was about 0. 2
The chips to which glue had been applied were
then spread out to form a mat and press-molded for
3.4 min at a temperature of 180~C with a press time
30 factor of 10 sec/mm to give a particle board. The
resultant particle board had the following parameters:

Thickness: 20.4 mm
Density: 650 kg/m3
Weight per m2: about 13.3 kg
Flexural strength: about 24 N/mm2
Transverse tensile strength (V 20): about 0. 42 N/mm2
Transverse tensile strength (V 100): about 0.18 N/mm2

CA 022~6398 1998-11-27

WO 97/46635 - 7 - PCT/EP97/02780

Thickness swelling (2 h): about 5.5%

The finished particle board can be used as a
furniture board in dry and damp areas, and also
externally as in the DIN Standards 68761 (Parts 1 and
4), 68762, 68763 and 68800.
The fire resistance of the particle board was
tested by directing the full flame of a bunsen burner
at a distance of 13.5 cm onto the surface of the board,
as a result of which the temperature prevailing there
was from 800 to 1000~C. Flame application for 5 min did
not ignite the particle board. All that was observed
was surface carbonization; very little smoke was
generated. The particle board fulfilled the
requirements of the DIN 4102 Standard.

Example 2:
Wheat straw was comminuted and separated into
fibers with a length of from 4 to 8 mm, a width of from
0.5 to 2 mm and a thickness of about 0.15 mm. These
straw fibers were mixed in a screw mixer with a fire-
protection agent in a solution of the following
composition:

21 parts by weight of ammonium sulfate,
5.4 parts by weight of borax,
3 parts by weight of trisodium phosphate,
0.6 parts by weight of sodium metasilicate,
70 parts by weight of water.
The ratio of the weight of the added solution
of the fire-protection agent to the dry weight of the
straw fibers was 0.67.
The impregnated straw fibers were then freed
from excess solution of the fire-protection agent in a
dewatering screw device and then dried to a residual
moisture content of about 4%.

CA 022~6398 l998-ll-27

WO 97/46635 - 8 - PCT/EP97/02780


PMDI resin was sprayed onto these straw fibers
in such a way that the ratio of the weight of the PMDI
resin to the dry weight of the straw fibers was 0. 06.
The impregnated and glued straw fibers were
spread out to form a mat, heated in a preheating
station to a core temperature of about 60~C and then
press-molded for 4.4 min at a temperature of 200~C and
with a press time factor of 15 sec/mm, to give a
fiberboard. The finished fiberboard had the following
parameters:

Thickness: 17.5 mm
Density: 550 kg/m3
Weight per m2: 9. 6 kg
The flame of a bunsen burner was also applied
to this fiberboard at a distance of 13.5 cm in such a
way that the temperature at the surface of the board
was from 800 to 1000~C. After the flame had been
applied for 5 min the board had not undergone any
change other than surface carbonization, which
developed without generation of flames. Very little
smoke generation was observed during this. The DIN 4102
Standard was again complied with.

Representative Drawing

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Administrative Status

For a clearer understanding of the status of the application/patent presented on this page, the site Disclaimer , as well as the definitions for Patent , Administrative Status , Maintenance Fee  and Payment History  should be consulted.

Administrative Status

Title Date
Forecasted Issue Date Unavailable
(86) PCT Filing Date 1997-05-28
(87) PCT Publication Date 1997-12-11
(85) National Entry 1998-11-27
Dead Application 2003-05-28

Abandonment History

Abandonment Date Reason Reinstatement Date
2002-05-28 FAILURE TO REQUEST EXAMINATION
2002-05-28 FAILURE TO PAY APPLICATION MAINTENANCE FEE

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $300.00 1998-11-27
Registration of a document - section 124 $100.00 1999-01-12
Registration of a document - section 124 $100.00 1999-01-12
Maintenance Fee - Application - New Act 2 1999-05-28 $100.00 1999-04-30
Maintenance Fee - Application - New Act 3 2000-05-29 $100.00 2000-05-24
Registration of a document - section 124 $100.00 2000-08-22
Maintenance Fee - Application - New Act 4 2001-05-28 $100.00 2001-05-24
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
NOPPER, HERBERT GEORG
Past Owners on Record
NOPPER, HERBERT G.
SCHMIDT, HUBERT F.
SUD-WEST-CHEMIE GMBH
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Cover Page 1999-02-15 1 57
Abstract 1998-11-27 1 19
Description 1998-11-27 10 389
Claims 1998-11-27 6 209
Assignment 1999-03-25 1 52
Correspondence 1999-02-22 1 2
Assignment 1999-01-12 3 105
PCT 1998-11-27 16 576
Assignment 1998-11-27 2 89
Assignment 2000-08-22 2 87
Fees 2001-05-24 1 48