CN101982305A - Preparation method of phosphate timber fire retardant and method for processing timber by using fire retardant - Google Patents
Preparation method of phosphate timber fire retardant and method for processing timber by using fire retardant Download PDFInfo
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- CN101982305A CN101982305A CN2010102680726A CN201010268072A CN101982305A CN 101982305 A CN101982305 A CN 101982305A CN 2010102680726 A CN2010102680726 A CN 2010102680726A CN 201010268072 A CN201010268072 A CN 201010268072A CN 101982305 A CN101982305 A CN 101982305A
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Abstract
The invention provides a preparation method of phosphate timber fire retardant and a method for processing timber by using the fire retardant. The fire retardant prepared by the invention is expansible annular phosphate timber fire retardant which contains an acid source, a carbon source and a gas resource, has the advantages of good expansiveness, compact carbon layer and certain intensity, and has good antiflaming effect proved by the measurement of an oxygen index and smoke density and the analysis of a dual cone calorimeter. The fire retardant is insoluble in water but soluble in organic solvent. The method for processing timber by fire retardant has the advantages of complete dipping, large dipping depth and lasting antiflaming effect, the dipping time is shorter than common dipping time, and time is saved.
Description
Technical field
The present invention relates to a kind of phosphate wood fire retardant preparation method and handle the method for timber with this fire retardant.
Background technology
Along with the fast development of economy, people are increasing to the demand of various construction materials.Wood materials is unique reproducible green, environment-friendly materials as one of four big construction materials (iron and steel, cement, timber, plastics).And because the natural characteristic of timber excellence is subjected to people's favor deeply.But wood-based product is inflammable, is the calamity source and the communication media of multiple fire.Not only daily life is brought potential danger, and limited the application of timber in a lot of fields.Therefore, inflammable timber being carried out flame treatment, in the hope of improvement with improve its some material wood property, make it obtain fully, utilize rationally, efficiently, is to adapt to the economic development requirement.
Have existed since ancient times for fire-retarding of wood, but fire-retarding of wood is studied existing many problems.The fire retardant commonly used for the treatment of of wood industry comprises mineral-type fire retardant and organic based flame retardant.Mineral-type fire retardant toxicity is little, cost is low but easily separate out, and influences the final flame retardant effect of timber.In recent years, along with perfecting of rules law, and the enhancing of people's environmental consciousness, the intumescent organic fire-retardant has been climbed up the arena of history, but the normal wood goods do not belong to the high consumption product, and the fire retardant cost is higher, has limited its extensive use.In addition, also there are destruction wood characteristics such as shortcomings such as toughness, intensity.
The fire-retardant research of timber is the research of a system engineering, and it comprises preliminary treatment (promptly improving permeability), fire retardant processing timber and the performance of timber, the problem of dry three aspects again of processing material.Fire retardant is handled timber and is comprised coating and flood two kinds of methods.Because some natural defects of timber, as exist pit to stop up, exist and invade shortcomings such as filling out thing, influence impregnating depth, and the molecular diameter size of fire retardant, influence treatment fluid and whether reach in the cell membrane, can be lastingly fire-retardant etc. factor.
Summary of the invention
At the problem that prior art exists, the object of the present invention is to provide a kind of phosphate wood fire retardant preparation method of good flame retardation effect, another object of the present invention provides the method that this fire retardant of a kind of usefulness is handled timber.
For achieving the above object, phosphate wood fire retardant preparation method of the present invention is specially:
1) in reaction vessel, add polyphosphoric acids and pentaerythrite according to mol ratio 2: 1～6: 1, add mass ratio 40%～70% carrene, and mass ratio be 10%～30% potash, adopt nitrogen protection, evenly stir, be warming up to 10 ℃～50 ℃, reaction 1h～3h;
2) continue to be warming up to 50 ℃～190 ℃ again, isothermal reaction 5h～10h;
3) cooled product, suction filtration is used washed with dichloromethane, and vacuum drying obtains cage shape phosphate white powder;
4) adding cage shape phosphate and melamine phosphate in 2: 1～4: 1 according to mol ratio, is that solvent evenly stirs with water, is warming up to 30 ℃～100 ℃ reaction 1h～5h, obtains ring-type phosphate;
5) ring-type phosphate is recrystallized the dry white powder fire retardant that gets in glacial acetic acid.
Further, the reaction vessel in the described step 1) has cooling and reflux device, hydrogen chloride gas retracting device.
Further, the pH of the cage shape phosphate in the described step 3) is 0.5～2.
Method with above-mentioned fire retardant processing timber is specially:
1) with pending timber through microwave treatment 10min～45min;
2) timber after will handling is put into process tank, and be 0.09MPa～0.25MPa with the process tank suction, keep 10min～20min, is to make solution in 1: 10～1: 60 with fire retardant and organic solvent by mass ratio, inject process tank, pressurization 0.1MPa～0.3MPa keeps 30min～50min, discharges solution;
3) timber after will flooding keeps 50 ℃～80 ℃ in vacuum drying chamber, and dry 8h～15h obtains flame treatment timber.
Further, the organic solvent described step 2) is a kind of in carrene, tetrachloromethane, carbon tetrachloride, dioxane, the toluene.
Utilize the inventive method to make to comprise the intumescent ring-type phosphate wood fire retardant of acid source, charcoal source, source of the gas, expansion character is good, and the charcoal layer is fine and close and have certain intensity, and by test oxygen index (OI), smoke density, and through the analysis of taper calorimeter, the flame retardant effect of fire retardant is good.The advantage that fire retardant is handled timber is: 1, dipping is complete, and impregnating depth is bigger, has lasting flame retardant effect; 2, dip time is shorter than common dipping, saves time.
The specific embodiment
The present invention will be further described below in conjunction with specific embodiment.
Embodiment one:
In being housed, the 500ml there-necked flask of condensation reflux unit adds polyphosphoric acids, pentaerythrite at 2: 1 according to mol ratio; methylene chloride 150ml; potash 15g, nitrogen protection, evenly stirring are warming up to 30 ℃ of reaction 45min; be warming up to 50 ℃ of reaction 4h again; cooling, suction filtration is used washed with dichloromethane; oven dry obtains cage shape phosphate powder.
In water, according to mol ratio 2: 1, with cage shape phosphate and melamine phosphate reaction, 60 ℃ of reactions of constant temperature 1h, cooling is filtered, and use the glacial acetic acid crystallization, and drying gets the ring-type phosphate powder.
Embodiment two:
In being housed, the 500ml there-necked flask of condensation reflux unit adds polyphosphoric acids, pentaerythrite at 3: 1 according to mol ratio; methylene chloride 200ml; potash 20g, nitrogen protection, evenly stirring are warming up to 50 ℃ of reaction 45min; be warming up to 85 ℃ of reaction 4h again; cooling, suction filtration is used washed with dichloromethane; oven dry obtains cage shape phosphate powder.
In water, according to mol ratio 2: 1, with cage shape phosphate and melamine phosphate reaction, 70 ℃ of reactions of constant temperature 1h, cooling is filtered, and use the glacial acetic acid crystallization, and drying gets the ring-type phosphate powder.
Embodiment three:
In being housed, the 500ml there-necked flask of condensation reflux unit adds polyphosphoric acids, pentaerythrite at 3: 1 according to mol ratio; methylene chloride 200ml; potash 20g, nitrogen protection, evenly stirring are warming up to 50 ℃ of reaction 1h; be warming up to 120 ℃ of reaction 4h again; cooling, suction filtration is used washed with dichloromethane; oven dry obtains cage shape phosphate powder.
In water, according to mol ratio 2: 1, with cage shape phosphate and melamine phosphate reaction, 85 ℃ of reactions of constant temperature 1h, cooling is filtered, and use the glacial acetic acid crystallization, and drying gets the ring-type phosphate powder.
Embodiment four:
The fire retarding wood treatment process may further comprise the steps: through microwave treatment 20min, the timber after the processing is put into process tank with ready timber, the vacuum pumping degree is 0.1MPa, keeping 15min, is to make solution, injection process tank at 1: 15 with fire retardant and organic solvent by mass ratio, pressurization 0.2MPa, keep 35min, discharge solution, timber keeps 50 ℃ in vacuum drying chamber, dry 8h obtains flame treatment timber.
Embodiment five:
The fire retarding wood treatment process may further comprise the steps: through microwave treatment 20min, the timber after the processing is put into process tank with ready timber, the vacuum pumping degree is 0.1MPa, keeping 15min, is to make solution, injection process tank at 1: 40 with fire retardant and organic solvent by mass ratio, pressurization 0.2MPa, keep 35min, discharge solution, timber keeps 80 ℃ in vacuum drying chamber, dry 13h obtains flame treatment timber.
The combustibility of the fire retarding wood among the present invention detects through following detection method
The be untreated method of material and flame treatment timber contrast of employing, according to GB/T 2406-93 plastics combustibility test method oxygen index method, test timber oxygen index (OI) result; According to the smoke density test method of burning of GB/T8627-2007 construction material or decomposition, test timber smoke density result; According to ISO5660-1, adopt the taper calorimeter at heat radiation power 50kW/m
2Condition under two kinds of timber are carried out fire resistance test.
The result is as shown in the table: show that untreated material is compared with the timber of flame treatment, oxygen index (OI) is lower, and smoke density is bigger, and the big more fire resistance of the concentration of fire retardant is good more.And draw through the analysis of taper calorimeter, the HRR peak value and the total heat burst size of flame treatment timber all greatly reduce.
The foregoing description only is used for that the present invention will be described, does not constitute the restriction to the claim scope, and other alternative means that it may occur to persons skilled in the art that are all in claim scope of the present invention.
Claims (5)
1. phosphate wood fire retardant preparation method is characterized in that, this method is specially:
1) in reaction vessel, add polyphosphoric acids and pentaerythrite according to mol ratio 2: 1～6: 1, add mass ratio and be 40%～70% carrene, and mass ratio be 10%～30% potash, adopt nitrogen protection, evenly stir, be warming up to 10 ℃～50 ℃, reaction 1h～3h;
2) continue to be warming up to 50 ℃～190 ℃ again, isothermal reaction 5h～10h;
3) cooled product, suction filtration is used washed with dichloromethane, and vacuum drying gets cage shape phosphate white powder;
4) adding cage shape phosphate and melamine phosphate in 2: 1～4: 1 according to mol ratio, is that solvent evenly stirs with water, is warming up to 30 ℃～100 ℃ reaction 1h～5h, gets ring-type phosphate;
5) ring-type phosphate is recrystallized the dry white powder fire retardant that gets in glacial acetic acid.
2. phosphate wood fire retardant preparation method as claimed in claim 1 is characterized in that the reaction vessel in the described step 1) has cooling and reflux device and hydrogen chloride gas retracting device.
3. phosphate wood fire retardant preparation method as claimed in claim 1 is characterized in that, the pH of the cage shape phosphate in the described step 3) is 0.5～2.
4. handle the method for timber with fire retardant, this method is specially:
1) with pending timber through microwave treatment 10min～45min;
2) timber after will handling is put into process tank, and be 0.09MPa～0.25MPa with the process tank suction, keep 10min～20min, is to make solution in 1: 10～1: 60 with fire retardant and organic solvent by mass ratio, inject process tank, pressurization 0.1MPa～0.3MPa keeps 30min～50min, discharges solution;
3) timber after will flooding keeps 50 ℃～80 ℃ in vacuum drying chamber, and dry 8h～15h obtains flame treatment timber.
5. fire retardant as claimed in claim 4 is handled the method for timber, it is characterized in that described step 2) in organic solvent be a kind of in carrene, tetrachloromethane, carbon tetrachloride, dioxane, the toluene.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102490227A (en) * | 2011-12-02 | 2012-06-13 | 朱江福 | Preparation process for mould-proof bamboo floor boards |
| CN103158181A (en) * | 2013-02-25 | 2013-06-19 | 东北林业大学 | Multifunctional wood inflaming retarding agent and method for preparing smoke suppressing and inflaming retarding pinus sylvestris solid wood by utilizing of multifunctional wood inflaming retarding agent |
| CN105538451A (en) * | 2016-01-28 | 2016-05-04 | 河南森远科技有限公司 | Method for preparing phosphorous-nitrogen synergistic wood fire retardant |
| CN105643743A (en) * | 2016-01-28 | 2016-06-08 | 河南森远科技有限公司 | Preparation method of wood fire retardant with synergized multiple elements of phosphorus, nitrogen and boron |
| CN108911613A (en) * | 2018-06-13 | 2018-11-30 | 合肥永泰新型建材有限公司 | A kind of board of low thermal conductivity and preparation method thereof |
| CN110172751A (en) * | 2019-05-18 | 2019-08-27 | 孔令孝 | A kind of carbon fibre and its carbonization method |
| CN110499549A (en) * | 2019-05-18 | 2019-11-26 | 孔令孝 | A kind of carbon fibre and its method using Lyocell fiber preparation |
| CN112549225A (en) * | 2020-11-28 | 2021-03-26 | 无锡市森泰木制品有限公司 | Wood processing method |
| CN117106332A (en) * | 2023-10-23 | 2023-11-24 | 中国林业科学研究院木材工业研究所 | Flame-retardant amino resin coating for repairing cracks of carbon layer as well as preparation method and application thereof |
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| CN1624074A (en) * | 2004-10-27 | 2005-06-08 | 华东理工大学 | Fire-retarded material of polypentaerythritol kind phosphate ester melamine salt expended type and its preparation process |
| CN101121892A (en) * | 2006-08-09 | 2008-02-13 | 上海高技企业发展公司 | Expansion type flame-retardant and its preparation method |
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| US4520152A (en) * | 1977-09-06 | 1985-05-28 | General Electric Company | Flame retardant composition of polyphenylene ether, styrene resin and cyclic phosphonate |
| CN1624074A (en) * | 2004-10-27 | 2005-06-08 | 华东理工大学 | Fire-retarded material of polypentaerythritol kind phosphate ester melamine salt expended type and its preparation process |
| CN101121892A (en) * | 2006-08-09 | 2008-02-13 | 上海高技企业发展公司 | Expansion type flame-retardant and its preparation method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102490227A (en) * | 2011-12-02 | 2012-06-13 | 朱江福 | Preparation process for mould-proof bamboo floor boards |
| CN103158181A (en) * | 2013-02-25 | 2013-06-19 | 东北林业大学 | Multifunctional wood inflaming retarding agent and method for preparing smoke suppressing and inflaming retarding pinus sylvestris solid wood by utilizing of multifunctional wood inflaming retarding agent |
| CN105538451A (en) * | 2016-01-28 | 2016-05-04 | 河南森远科技有限公司 | Method for preparing phosphorous-nitrogen synergistic wood fire retardant |
| CN105643743A (en) * | 2016-01-28 | 2016-06-08 | 河南森远科技有限公司 | Preparation method of wood fire retardant with synergized multiple elements of phosphorus, nitrogen and boron |
| CN105538451B (en) * | 2016-01-28 | 2017-03-22 | 河南森远科技有限公司 | Method for preparing phosphorous-nitrogen synergistic wood fire retardant |
| CN105643743B (en) * | 2016-01-28 | 2017-03-29 | 河南森远科技有限公司 | A kind of phosphorus nitrogen boron multielement cooperates with the preparation method of wood fire retardant |
| CN108911613A (en) * | 2018-06-13 | 2018-11-30 | 合肥永泰新型建材有限公司 | A kind of board of low thermal conductivity and preparation method thereof |
| CN110172751A (en) * | 2019-05-18 | 2019-08-27 | 孔令孝 | A kind of carbon fibre and its carbonization method |
| CN110499549A (en) * | 2019-05-18 | 2019-11-26 | 孔令孝 | A kind of carbon fibre and its method using Lyocell fiber preparation |
| CN112549225A (en) * | 2020-11-28 | 2021-03-26 | 无锡市森泰木制品有限公司 | Wood processing method |
| CN117106332A (en) * | 2023-10-23 | 2023-11-24 | 中国林业科学研究院木材工业研究所 | Flame-retardant amino resin coating for repairing cracks of carbon layer as well as preparation method and application thereof |
| CN117106332B (en) * | 2023-10-23 | 2023-12-29 | 中国林业科学研究院木材工业研究所 | Flame-retardant amino resin coating for repairing cracks of carbon layer as well as preparation method and application thereof |
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| CN101982305B (en) | 2012-11-21 |
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