# US 2018/0021975 A1 · Fire resistant wooden body and method for producing thereof

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- Number: US 2018/0021975 A1
- Document ID: US20180021975A1
- Status: Published application
- Kind: A1
- Application number: 15/548,105
- Filed: 2016-01-29
- Published: 2018-01-25
- Earliest claimed: 2015-02-02
- Assignees: Torcitura Padana S.p.A.; Zanolo S.p.A.
- Applicants: TORCITURA PADANA S.p.A.; ZANOLO S.p.A.
- Inventors: Alberto TONANI; Andrea NOVELLO; Calogero SIRNA; Simona PESARO
- Web page: https://patentgrep.com/patent/US20180021975A1

## CPC

- B27K 3/52: Impregnating agents containing mixtures of inorganic and organic compounds
- B01J 31/0257: {Phosphorus acids or phosphorus acid esters}
- B27K 3/16: Inorganic impregnating agents
- B27K 3/20: Compounds of alkali metals or ammonium
- B27K 3/346: {Grafting onto wood fibres (B27K3/156 takes precedence; macromolecular compounds derived from lignocellulosic materials C08H)}
- C08B 5/00: Preparation of cellulose esters of inorganic acids {, e.g. phosphates (rendering cellulose suitable for esterification C08B1/02)}
- C08H 8/00: Macromolecular compounds derived from lignocellulosic materials {(pretreatment thereof B27N)}
- C09K 21/12: containing phosphorus
- B27K 2240/30: Fireproofing
- B27K: PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR (applying liquids or other fluent materials to surfaces in general B05; coating wood or similar material B44D); CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21)
- C08H: DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS (polysaccharides C08B; natural rubber C08C; natural resins or their derivatives C09F; bituminous materials C10)
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE

## Abstract

A method for sulphation and phosphorylation of a wooden body to impart anti-flame properties to the substrate wherein at least one phosphonic acid of the formula (I) is used PO(OH)2—R—PO(OH)2 as a catalyst for sulphation and phosphorylating agent, and the relative wooden body.

## Claims

### Claim 1

A method for sulphation and phosphorylation of a wooden body to impart anti-flame properties to the wooden body comprising the following operations:
i) providing a wooden body, preferably a dried wooden body;
ii) preparing a sulphation and phosphorylation solution, preferably under heated conditions, the sulphation and phosphorylation solution comprising water, ammonium sulphamate, urea and at least one compound of the formula (I):
PO(OH)2—R—PO(OH)2 (I)
wherein
R represents a linear or branched, substituted or unsubstituted C1-10, preferably C1-5, alkyl group; an N(R1) group; a R2N(R3)R4 group;
R1 represents H, a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
R2 and R4 independently represent a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
R3 represents a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group; a R5N(R6)R7 group;
R5 and R7 independently represent a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
R6 represents a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group; a R8N(R9)R10 group;
R8, R9 and R10 independently represent a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
with the proviso that the number of —PO(OH)2 groups in the general formula (I) is not greater than 5;
iii) immersing the wooden body into the sulphation and phosphorylation solution, preferably at a pressure higher than atmospheric pressure;
iv) extracting the wooden body from the sulphation and phosphorylation solution;
v) maintaining the wooden body at a temperature between 110° and 175° C. for a period of time between 1 minute and 5 hours, obtaining at the end a sulphated and phosphorylated wooden body with anti-flame properties.

### Claim 2 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein before operation v) the wooden body extracted from the sulphation and phosphorylation solution is subjected to a dripping and heat drying operation, preferably at a temperature between 70 and 90° C.

### Claim 3 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein at the end of the operation v) the wooden body is subjected to a washing operation, preferably under heated condition, and heat drying, preferably at a temperature between 70 and 90° C.

### Claim 4 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein before operation iii) the wooden body is subjected to an outgassing operation at a pressure lower than atmospheric pressure.

### Claim 5 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the sulphation and phosphorylation solution is prepared by mixing, in the following order, water, urea, at least one compound of formula (I) and ammonium sulphamate.

### Claim 6 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the sulphation and phosphorylation solution contains:
water in a quantity between 80 and 25% w/w, preferably between 50 and 60% w/w,
urea in a quantity between 10 and 30% w/w, preferably between 10 and 20% w/w,
at least one compound of formula (I) in an quantity between 5 and 30% w/w, preferably between 10 and 20% w/w, and
ammonium sulphamate in a quantity between 5 and 30% w/w, preferably between 8 and 15% w/w.

### Claim 7 (depends on 1)

The method of sulphation and phosphorylation according to claim 1, wherein when any one of the groups R, R1, R2, R3, R4, R5, R6, R7, R8, R9, R10, of the general formula (I), if present, represents a substituted alkyl group, the one or more substituents are independently selected from —OH, —COOH, —PO(OH)2, —NH2, —NHR11, —NR12R13, —Cl, —Br, —F, wherein
R11, R12 and R13 independently represent a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group.

### Claim 8 (depends on 7)

The method for sulphation and phosphorylation according to claim 7, wherein when any one of the groups R11, R12 and R13 of the general formula (I), if present, represents a substituted alkyl group, the one or more substituents are represented by the —PO(OH)2 group.

### Claim 9 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the groups R2, R4, R5 and R8, if present, independently represent an unsubstituted alkyl group.

### Claim 10 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein when the groups R3, R6, R7, R9 and R10, if present, independently represent a substituted alkyl group, the one or more substituents are represented by the —PO(OH)2 group.

### Claim 11 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the at least one phosphonic compound of formula (I) is selected from: 1-hydroxyethan-1,1-bisphosphonic acid, hydroxyethyl-imino-bis-(methylene-phosphonic) acid, amino-tris-(methylene phosphonic) acid, ethylene diamine tetra-(methylene phosphonic) acid, diethylentriamine-penta-(methylene phosphonic) acid, (1-aminoethylidene) bisphosphonic acid, oxidronic acid, pamidronic acid, alendronic acid, (1-hydroxy-2-methyl-1-phosphonopropyl) phosphonic acid, (aminomethylene) bisphosphonic acid, 1-hydroxypentane-1,1-bisphosphonic acid, [(2-hydroxypropan-1,3-diyl) bis(nitrilodimethane-diyl)] tetrakis-phosphonic acid, clodronic acid, (difluoromethylene) bisphosphonic acid, (dibromomethylene) bisphosphonic acid, (hydroxymethan) bisphosphonic acid.

### Claim 12 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the wooden body essentially consists of cellulose, hemicellulose and lignin.

### Claim 13 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the sulphated and phosphorylated wooden body has an L.O.I. between 30 and 90, more preferably between 60 and 80.

### Claim 14 (depends on 1)

The method for sulphation and phosphorylation according to claim 1, wherein the sulphated and phosphorylated wooden body has physical properties essentially equal to those of an untreated wooden body.

### Claim 15 (depends on 1)

A wooden body with anti-flame properties obtained by implementing the method according to claim 1.

### Claim 16

Use of a compound of formula (I):
PO(OH)2—R—PO(OH)2 (I)
wherein
R represents a linear or branched, substituted or unsubstituted C1-10, preferably C1-5, alkyl group; an N(R1) group; a R2N(R3)R4 group;
R1 represents H, a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
R2 and R4 independently represent a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
R3 represents a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group; a R5N(R6)R7 group;
R5 and R7 independently represent a linear or branched, substituted or unsubstituted C1-3, preferably C1-3, alkyl group.
R6 represents a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group; a R8N(R9)R10; group;
R8, R9 and R10 independently represent a linear or branched, substituted or unsubstituted C1-5, preferably C1-3, alkyl group;
with the proviso that the number of —PO(OH)2 groups in the general formula (I) is not greater than 5;
in a method for sulphation and phosphorylation of a wooden body, the compound of formula (I) acting as a catalytic agent in the sulphation reaction and a phosphorylating agent.