CN101805619B - Method for preparing nitrogen-phosphorus fire retardant - Google Patents
Method for preparing nitrogen-phosphorus fire retardant Download PDFInfo
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- CN101805619B CN101805619B CN201010142916A CN201010142916A CN101805619B CN 101805619 B CN101805619 B CN 101805619B CN 201010142916 A CN201010142916 A CN 201010142916A CN 201010142916 A CN201010142916 A CN 201010142916A CN 101805619 B CN101805619 B CN 101805619B
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- ureaphil
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Abstract
The invention discloses a method for preparing a nitrogen-phosphorus fire retardant, comprising the following steps: concentrating urea phosphate mother liquor until the water loss reaches 32.04-32.14% to obtain urea phosphate mother liquor concentrate; evenly mixing the urea phosphate mother liquor concentrate and urea in a reactor according to the mass ratio of 1:0.15-0.3; sealing the reactor, injecting ammonia and maintaining pressure inside the reactor at 0.01-0.45MPa; raising temperature of the reactor to 100 DEG C at a speed of 8-10 DEG C/min and retaining the temperature for 10min; contribute raise the temperature to 150 DEG C at a speed of 3-4 DEG C/min and retaining the temperature for 30-90min; afterwards continuing raising the temperature to 220-275 DEG C at a speed of 5-6 DEG C/min and retaining the temperature for 60-120min; then cooling to obtain the nitrogen-phosphorus fire retardant. The product prepared by the method features good appearance, high purity, simple technology, easy realization of industrialized production, small equipment investment and wide source of raw materials.
Description
Technical field
The invention belongs to chemical technology field, relate in particular to a kind of preparation method of fire retardant.
Background technology
Nitrogen-phosphorus fire retardant is the fire retardant of a kind of without halide efficiently of developing rapidly both at home and abroad in recent years, and the polymerization degree is insoluble in water greater than 20 nitrogen-phosphorus fire retardant, and decomposition temperature generally is higher than 250 ℃; And nitrogen-phosphorus content is high, and water absorbability is little, and chemicalstability is good; Toxicity is low, and smoke suppressing effect is good, can be used as plastics, rubber, fire-retardant for fibre; The fire prevention of preparation expanding fire-proof paint and some facilities is handled, and is a kind of environment friendly flame retardant.
Along with improving constantly of fast development of national economy and people's living standard, construction and decoration is ascendant trend year by year with the ratio of timber total flow.But undressed timber and goods thereof belong to red label goods.According to the fire statistics data analysis, in the fire failure of countries in the world, building fire accounts for the first place, and the building fire cause is different.But the intensity of a fire enlarges, loss of life and personal injury all with the buildings interior decoration in the flammable inflammable materials such as wood materials that use direct relation is arranged.Timber is carried out fire-retardant finish, is one of effective way that reduces fire failure.Nitrogen-phosphorus fire retardant is to be used to improve the material fire resistance; Promptly stop material to be ignited and suppress the processing aid of propagation of flame, be widely used in the fire-retardant of synthetic and natural macromolecular material (comprising plastics, rubber, fiber, timber, paper, paint, coating etc.).Contain with phosphorus, nitrogen is the polyphosphoric acid salt wood fire retardant of ignition-proof element; Not halogen-containing, need not adopt the antimony synergist, when the timber of using this fire retardant to handle receives heat-flash or burning; Decompose and generate polyphosphoric acid; Impel the carbonization of wood, generate layer of even porous carbonaceous foam layer on its surface, this foam layer is heat insulation, oxygen barrier, press down hood.But common in the market polyphosphoric acid salt wood fire retardant mainly is an ammonium polyphosphate, and its cost is higher, and production technique is more complicated also.
Ureaphil is that phosphoric acid by wet process and urea reaction make, and behind phosphoric acid by wet process and the urea reaction, can make Ureaphil through concentrated, crystallization, separation, drying step, and its chemical formula is: H
3PO
4CO (NH
2)
2Simultaneously, this process has a large amount of Ureaphil crystalline mother solution to produce that (the Ureaphil mother liquor is the tawny thick liquid, and boiling point is 110 ℃, and pH is 3-4, water cut 40-55%, N content: 9-12%, P
2O
5Content: 20-25%).Mother liquor processing method is to deliver to the fertilizer system recoveries to use at present, can't effective constituent wherein be made full use of.The recovery of mass crystallization mother liquor, deep processing are present production of urea phosphate industry urgent problems.Chinese patent publication number CNCN101121277 was on 02 13rd, 2008; Disclosing " a kind of nitrogen--phosphorus efficiency expansion type wood fire retardant and preparation method thereof ", is to utilize the Ureaphil mother liquor to stir behind the back underpressure distillation 1.5-2h mother liquor water cut less than 8% adding Fe, Mg, Ga, Al metals ion activator and boric acid; Crystalline mother solution after dewatering is put into the polymerization reaction kettle polymerization that electric mixer is housed and got.Because need to add activator, thus complex process, to adopt in the polymerization reaction kettle with electronic whisking appliance, facility investment is big, and production cost is high.
Summary of the invention
The apparent sex character of a kind of product that the objective of the invention is to overcome above-mentioned shortcoming and provide is good, and purity is high, technology is simple and easy to industriallization, the preparation method of the nitrogen-phosphorus fire retardant that facility investment is few, raw material sources are wide.
The object of the invention and solve its technical problem underlying and adopt following technical scheme to realize.
The preparation method of a kind of nitrogen-phosphorus fire retardant of the present invention may further comprise the steps:
(1) is about 32% with the Ureaphil mother liquor being concentrated to percentage of water loss, gets Ureaphil mother liquor enriched material;
(2) be 1 by Ureaphil mother liquor enriched material with the urea quality ratio: 0.15-0.3 mixes in reactor drum, after the sealing, feeds ammonia, makes reactor pressure maintain 0.01-0.04MPa; Speed with 8-10 ℃/min makes reactor drum be raised to 100 ℃, insulation 10min; With the speed of 3-4 ℃/min, continue to be warmed up to 150 ℃, soaking time is 30-90min; Speed with 5-6 ℃/min continues to be warmed up to 220-275 ℃ subsequently, and soaking time is 60-120min, promptly gets after the cooling.
The preparation method of above-mentioned a kind of nitrogen-phosphorus fire retardant, wherein: the Ureaphil mother liquor is 80 ℃ in temperature, underpressure distillation 2h gets Ureaphil mother liquor enriched material.
The present invention compared with prior art has tangible beneficial effect, can know from above technical scheme: present method is a raw material with Ureaphil mother liquor and urea; Do not add any activator, in the ammonia atmosphere, through the temperature programming of syllogic; Cooling makes nitrogen-phosphorus fire retardant, and technology is simple, and facility investment is few; Raw material sources are wide, and raw material, product and thermal decomposition product thereof are nontoxic or low toxicity.It is good that the product of preparation has apparent sex character, the purity advantages of higher.Not only solved the refuse reclamation problem of phosphoric acid by wet process mother liquor well, and the fire retardant that makes has using value.
Embodiment
Embodiment 1:
(1) take by weighing 156g Ureaphil mother liquor in Rotary Evaporators, underpressure distillation (maintaining the temperature at 80 ℃) 2h gets Ureaphil mother liquor enriched material 106g, and concentrating the back percentage of water loss is 32.05%;
(2) get 30g Ureaphil mother liquor enriched material and 4.5 gram urea mix in reaction kettle, after the sealing, feed ammonia, keeping the still internal pressure is 0.02MPa.Speed with 10 ℃/min is warmed up to 100 ℃, behind the insulation 10min, with the speed of 4 ℃/min, continues to be warmed up to 150 ℃, insulation 90min, and the speed with 6 ℃/min continues to be warmed up to 250 ℃ subsequently, insulation 120min, the cooling back obtains nitrogen-phosphorus fire retardant 6.0 grams.
Through detecting: total nitrogen content 12.1%, total phosphorus pentoxide content 56.8%, N: P
2O
5=1: 4.69, the polymerization degree 32.05.Adopt this fire retardant to handle the timber test block, the limiting oxygen index determination value reaches 64%, can detect through the fire-retardant B1 level of material of construction.
Embodiment 2:
(1) take by weighing 156.5g Ureaphil mother liquor in Rotary Evaporators, underpressure distillation (maintaining the temperature at 80 ℃) 2h gets Ureaphil mother liquor enriched material 106.2g, and concentrating the back percentage of water loss is 32.14%;
(2) get 30g Ureaphil mother liquor enriched material and 6 gram urea mix in reaction kettle, after the sealing, feed ammonia, keeping the still internal pressure is 0.01MPa; Speed with 8 ℃/min is warmed up to 100 ℃, behind the insulation 10min, with the speed of 3 ℃/min; Continue to be warmed up to 150 ℃, insulation 60min, the speed with 5 ℃/min continues to be warmed up to 235 ℃ subsequently; Insulation 90min, cooling obtains nitrogen-phosphorus fire retardant 6.3 grams.
Through detecting: total nitrogen content 12.5%, total phosphorus pentoxide content 55.5%, N: P
2O
5=1: 4.44, the polymerization degree 30.05.Adopt this fire retardant to handle the timber test block, the limiting oxygen index determination value reaches 60%, can detect through the fire-retardant B1 level of material of construction.
Embodiment 3:
(1) take by weighing 157g Ureaphil mother liquor in Rotary Evaporators, underpressure distillation (maintaining the temperature at 80 ℃) 2h gets Ureaphil mother liquor enriched material 106.6g, and concentrating the back percentage of water loss is 32.10%;
(2) get 30g Ureaphil mother liquor enriched material and 7.5 gram urea mix in reaction kettle, after the sealing, feed ammonia, keeping the still internal pressure is 0.03MPa; Speed with 8 ℃/min is warmed up to 100 ℃, behind the insulation 10min, with the speed of 4 ℃/min, continues to be warmed up to 150 ℃, insulation 30min, and the speed with 6 ℃/min continues to be warmed up to 220 ℃ subsequently, insulation 60min, cooling obtains nitrogen phosphorus fire retardant 6.34 grams.
Through detecting: total nitrogen content 12.7%, total phosphorus pentoxide content 56.2%, N: P
2O
5=1: 4.43, the polymerization degree 30.05.Adopt this fire retardant to handle the timber test block, the limiting oxygen index determination value reaches 61%, can detect through the fire-retardant B1 level of material of construction.
Embodiment 4
(1) take by weighing 155.7g Ureaphil mother liquor in Rotary Evaporators, underpressure distillation (maintaining the temperature at 80 ℃) 2h gets Ureaphil mother liquor enriched material 105.8g, and concentrating the back percentage of water loss is 32.04%;
(2) get 30g Ureaphil mother liquor enriched material and 9 gram urea mix in reaction kettle, after the sealing, feed ammonia, keeping the still internal pressure is 0.04MPa.Speed with 9 ℃/min is warmed up to 100 ℃, behind the insulation 10min, with the speed of 3 ℃/min, continues to be warmed up to 150 ℃, insulation 70min, and the speed with 5 ℃/min continues to be warmed up to 275 ℃ subsequently, insulation 1.2h, cooling obtains nitrogen-phosphorus fire retardant 5.4 grams.
Through detecting: total nitrogen content 12.4%, total phosphorus pentoxide content 56.3%, N: P
2O
5=1: 4.54, the polymerization degree 31.05.Adopt this fire retardant to handle the timber test block, the limiting oxygen index determination value reaches 63%, can detect through the fire-retardant B1 level of material of construction.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction; Anyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (2)
1. the preparation method of a nitrogen-phosphorus fire retardant may further comprise the steps:
(1) is 32.04-32.14% with the Ureaphil mother liquor being concentrated to percentage of water loss, gets Ureaphil mother liquor enriched material;
(2) be 1 by Ureaphil mother liquor enriched material with the urea quality ratio: 0.15-0.3 mixes in reactor drum, after the sealing, feeds ammonia, makes reactor pressure maintain 0.01-0.04MPa; Speed with 8-10 ℃/min makes reactor drum be raised to 100 ℃, insulation 10min; With the speed of 3-4 ℃/min, continue to be warmed up to 150 ℃, soaking time is 30-90min; Speed with 5-6 ℃/min continues to be warmed up to 220-275 ℃ subsequently, and soaking time is 60-120min, promptly gets after the cooling.
2. the preparation method of a kind of nitrogen-phosphorus fire retardant as claimed in claim 1, wherein: the Ureaphil mother liquor is 80 ℃ in temperature, underpressure distillation 2h, Ureaphil mother liquor enriched material.
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| CN201010142916A CN101805619B (en) | 2010-04-09 | 2010-04-09 | Method for preparing nitrogen-phosphorus fire retardant |
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| CN201010142916A CN101805619B (en) | 2010-04-09 | 2010-04-09 | Method for preparing nitrogen-phosphorus fire retardant |
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| CN101805619A CN101805619A (en) | 2010-08-18 |
| CN101805619B true CN101805619B (en) | 2012-10-03 |
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| CN102786742A (en) * | 2011-05-16 | 2012-11-21 | 山东道恩高分子材料股份有限公司 | Nitrogen and phosphorus system halogen-free flame retardation TPV material |
| CN106589623A (en) * | 2016-12-16 | 2017-04-26 | 江苏昌达环保科技有限公司 | Environment-friendly flame-retardant rubber floor and preparation method thereof |
| CN115651207B (en) * | 2022-10-14 | 2023-07-07 | 江西省安安科技有限公司 | In-situ polymerization flame retardant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1160305A2 (en) * | 2000-06-03 | 2001-12-05 | Semmelroth-Consulting GmbH | Process for the production of a fireproofing agent for combustible materials |
| CN101121277A (en) * | 2007-07-27 | 2008-02-13 | 贵州宏福实业开发有限总公司 | Nitrogen-phosphorus high-efficient expansion type wood flame-proof agent and its preparation method |
-
2010
- 2010-04-09 CN CN201010142916A patent/CN101805619B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1160305A2 (en) * | 2000-06-03 | 2001-12-05 | Semmelroth-Consulting GmbH | Process for the production of a fireproofing agent for combustible materials |
| CN101121277A (en) * | 2007-07-27 | 2008-02-13 | 贵州宏福实业开发有限总公司 | Nitrogen-phosphorus high-efficient expansion type wood flame-proof agent and its preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 李天祥等.用磷酸脲结晶母液合成的氮-磷高效膨胀型木材阻燃剂的性能研究.《贵州工业大学学报（自然科学版）》.2007,第36卷(第4期),第26-29页. * |
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