CN107474247A - A kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant - Google Patents
A kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant Download PDFInfo
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Abstract
The invention belongs to functional high molecule material application field, and in particular to a kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant.This method prepares phosphorous intermediate, activated afterwards with potassium rhodanide using neopentyl glycol and POCl3 as raw material, then intermediate polyethyleneimine nitrogenous with macromolecular reaction, obtains the powdered phosphorus nitrogen synergistic high molecular weight flame retardant of yellowish-brown.The fire retardant is water-soluble, and molecular weight can be adjusted according to demand, good with high polymer material compatibility, can improve the fire resistance of material.The fire retardant can effectively solve the problems, such as that common phosphorus nitrogen synergistic type fire retardant is not soluble in water, can effectively disperse when being prepared applied to materials such as water-blown polyurethanes, be not easy the migration precipitation from material, overcome the problem of material mechanical performance is deteriorated.Manufacturing condition of the present invention is easy, product purity is high, easy to use.
Description
Technical field
The present invention relates to a kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant.Function of dominant high polymer material should
Use field.
Background technology
As high polymer material is in the application of the every field such as chemical industry, building, aviation, automobile, electrical equipment, especially with good
Good insulation, the increase of heat-insulated, sound insulation function foamed material application amount, its flammable problem become the emphasis of people's research.
Polyurethane, polyethylene Polymer material is commonly used, containing a large amount of flammable hydrocarbon segments, limited oxygen index is low, especially
After foamed material is prepared as, specific surface area increase, density is small, has higher air circulation, not only easily burns, also hold
Easily a large amount of toxic smogs are produced in combustion.Once on fire, fire extinguishing is difficult, easily causes serious disaster and loss.
The fire resistance of high polymer material is improved, mainly forms compound system by adding fire retardant into material, or
By reaction, the methods of anti-flammability group is introduced directly into macromolecular chain, is realized.Because reactive flame retardant easily changes
The machinery of material, processing characteristics, thus at present still based on additive flame retardant.Element with anti-flammability mainly include Al,
N, P, Br, Cl, Si etc., wherein fire retardant containing Al is mostly inorganic type, the fire retardant containing other ignition-proof elements is then based on organic type.
China is the maximum fire retardant consumption market in the current whole world, annual consumption more than 300,000 tons, usage amount it is most for bromine system it is fire-retardant
Agent.Although bromide fire retardant flame retarding efficiency is high, it also increasingly shows in the shortcomings that environmental protection and secure context.Due to its fire-retardant machine
Reason is that gas phase is fire-retardant mostly, and a large amount of smog, corrosive gas and toxic gas, part bromine system can be produced when playing fire retardation
Fire retardant can also discharge the hydrogen halide harmful to human body and environment Ji bioxin (more bromo dibenzo in combustion
Bioxin and PBDF), and most bromide fire retardants are not easy to decompose, and easily accumulate in the environment, to ring
Border and biology cause long-term hazards.Therefore, fire retardant is progressively sent out to directions such as environmental protection, low toxicityization, high efficiency, multifunctions
Exhibition.
Phosphorus system and nitrogenated flame retardant are current low cigarette, the representatives of low-poison and combustion-resisting agent, have preferable environmental-protecting performance.Especially
Using phosphorus, nitrogen synergistic type as the expansion type flame retardant of representative, charcoal source is had concurrently, acid source is gentle comes from one, not only environmental-protecting performance is good,
It can also prevent to burn from different approaches, there is excellent flame retarding efficiency.But these fire retardants are mostly inorganic type and organic
Type small molecule, for high polymer material it is fire-retardant when, easily occur causing the mechanical property of materials, heat steady because compatibility is bad
Qualitative the problems such as declining, be exudative.Thus, current fire retardant also develops to producing high-molecular, to solve small molecule fire retardant
The problem of with high polymer material poor compatibility, easy to migrate, influence material mechanical performance and mechanical strength.On the other hand, macromolecule
Expansion type flame retardant is typically difficult to be dissolved in solvent, is easily separated when being added in high polymer material, causes fire resistance
Skewness.Therefore, exploitation is soluble, and the expansion type flame retardant for being easy to add and using is also current research direction.
Thus, plan passes through phosphorous intermediate and the nitrogenous intermediate reaction of macromolecule, prepares with good flame retarding efficiency,
With good high polymer material compatibility, the nitrogen phosphorus synergistic high molecular weight flame retardant of safety and environmental protection, by controlling fire retardant
Structure, certain water solubility is made it have, convenient use, adjusts its molecular weight according to demand, suitable for a variety of high polymer materials
It is fire-retardant.
The content of the invention
It is an object of the invention to provide a kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant.
The technical scheme is that：First using neopentyl glycol and POCl3 as raw material, in 85 DEG C of backflows in solvent I
Reaction 4~10 hours, revolving, drying obtain the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl in oneself
Phosphate, afterwards by the dioxy phosphas of 5,5- dimethyl -2- chloro- 1,3,2- in oneself acyl phosphate and potassium rhodanide in solvent II in
60 DEG C of back flow reactions 4~10 hours, are filtered to remove potassium chloride, obtain 5,5- dimethyl -2- isothiocyanos -1,3,2- dioxies phospha oneself
Interior acyl phosphate filtrate, then the nitrogenous intermediate polyethyleneimine of macromolecular is added in filtrate, after reacting 4~12 hours, product
Through filtering, washing, drying and processing, yellowish-brown powder, as phosphorus nitrogen synergistic high molecular weight flame retardant are obtained.
The present invention relates to a kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant, the fire retardant is water-soluble,
Molecular weight can be adjusted according to demand, good with polymer-polymer miscibility, can improve the fire resistance of material.The fire retardant energy
Effectively solve the problems, such as that common phosphorus nitrogen synergistic type fire retardant is not soluble in water, can have when being prepared applied to materials such as water-blown polyurethanes
Effect is scattered, is not easy the migration precipitation from material, overcomes the problem of material mechanical performance is deteriorated.Manufacturing condition letter of the present invention
Just, product purity is high, easy to use.
Specifically, the processing step of this method and condition are as follows：
(1) first by neopentyl glycol (NPG) and POCl3 (POCl3) be dissolved in solvent I, in 85 DEG C of back flow reactions 4~
10 hours, revolving, drying obtained the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl phosphate in oneself；
(2) by the chloro- 1,3,2- dioxies phosphas of 5,5- dimethyl -2- obtained in step (1), oneself interior acyl phosphate is molten after
In the solvent II containing potassium rhodanide (KSCN), in 60 DEG C of back flow reactions 4~10 hours, potassium chloride is filtered to remove, obtains 5,5- bis-
Methyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
The nitrogenous intermediate polyethyleneimine (PEI) of macromolecular is added in filtrate, after reacting 4~12 hours, filters, dry to obtain yellowish-brown toner
Last shape phosphorus nitrogen synergistic water soluble polymer fire retardant；
Above-mentioned chemical equation is：
The structural formula of gained phosphorus nitrogen synergistic water soluble polymer fire retardant is：
N is the positive integer more than 0 in formula.
In above-mentioned preparation method, neopentyl glycol is 1 with POCl3 molar ratio:1~1:6, solvent I are dichloromethane
Any of alkane, acetone, 1,2- dichloroethanes, acetonitrile；The chloro- 1,3,2- dioxies phosphas of 5,5- dimethyl -2- acyl phosphoric acid in oneself
The molar ratio of ester and potassium rhodanide is 1:1, solvent II is any of acetone, 1,2- dichloroethanes；It is used poly-
Aziridine is branched chain type, and its weight average molecular weight is 600~60000Da；5,5- dimethyl -2- isothiocyano -1,3,2- dioxies
Oneself molar ratio of interior acyl phosphate and polyethyleneimine of phospha is 3:1~405:1, the substitution of polyethyleneimine surface amino groups
Spend for 50%~90%.
Embodiment
Following example will be explained in detail the operating method of the present invention, but cannot function as limitation of the invention.
Embodiment 1
(1) 10.4g neopentyl glycols and 9.3mL POCl3s are dissolved in 1,2- dichloroethanes first, it is anti-in 85 DEG C of backflows
Answer 10 hours, revolving, drying obtain the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl phosphoric acid in oneself
Ester；
(2) by the chloro- 1,3,2- dioxies phosphas of 18.5g5,5- dimethyl -2- obtained in step (1) acyl phosphoric acid in oneself after
Ester is dissolved in the acetone soln of the potassium rhodanide containing 9.7g, in 60 DEG C of back flow reactions 4 hours, is filtered to remove potassium chloride, is obtained 5,5- bis-
Methyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
The nitrogenous intermediate polyethyleneimine of macromolecular that 10g molecular weight is 600Da is added in filtrate, after reacting 6 hours, is filtered, drying
Obtain the powdered phosphorus nitrogen synergistic water soluble polymer fire retardant of yellowish-brown, surface amino groups substitution value 90%.
Embodiment 2
(1) 10.4g neopentyl glycols and 18.6mL POCl3s are dissolved in dichloromethane first, in 85 DEG C of back flow reactions 8
Hour, revolving, drying obtain the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl phosphate in oneself；
(2) by the chloro- 1,3,2- dioxies phosphas of 18.5g5,5- dimethyl -2- obtained in step (1) acyl phosphoric acid in oneself after
Ester is dissolved in 1 of the potassium rhodanide containing 9.7g, in 2- dichloroethane solutions, in 60 DEG C of back flow reactions 6 hours, is filtered to remove potassium chloride,
5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
It is the nitrogenous intermediate polyethyleneimine of 1800Da macromoleculars that 15g molecular weight is added in filtrate, after reacting 10 hours, is filtered, drying
Obtain the powdered phosphorus nitrogen synergistic water soluble polymer fire retardant of yellowish-brown, surface amino groups substitution value 75%.
Embodiment 3
(1) 10.4g neopentyl glycols and 37.2mL POCl3s are dissolved in acetone first, in 85 DEG C of back flow reactions 6 hours,
Revolving, drying obtain the phosphorous chloro- 1,3,2- dioxies phosphas of intermediate 5,5- dimethyl -2- of white acyl phosphate in oneself；
(2) by the chloro- 1,3,2- dioxies phosphas of 18.5g5,5- dimethyl -2- obtained in step (1) acyl phosphoric acid in oneself after
Ester is dissolved in 1 of the potassium rhodanide containing 9.7g, in 2- dichloroethane solutions, in 60 DEG C of back flow reactions 8 hours, is filtered to remove potassium chloride,
5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
It is the nitrogenous intermediate polyethyleneimine of 25000Da macromoleculars that 18g molecular weight is added in filtrate, after reacting 12 hours, is filtered, drying
Obtain the powdered phosphorus nitrogen synergistic water soluble polymer fire retardant of yellowish-brown, surface amino groups substitution value 70%.
Embodiment 4
(1) 10.4g neopentyl glycols and 55.8mL POCl3s are dissolved in 1,2- dichloroethanes first, it is anti-in 85 DEG C of backflows
Answer 4 hours, revolving, drying obtain the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl phosphoric acid in oneself
Ester；
(2) by the chloro- 1,3,2- dioxies phosphas of 18.5g5,5- dimethyl -2- obtained in step (1) acyl phosphoric acid in oneself after
Ester is dissolved in the acetone soln of the potassium rhodanide containing 9.7g, in 60 DEG C of back flow reactions 10 hours, is filtered to remove potassium chloride, is obtained 5,5- bis-
Methyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
It is the nitrogenous intermediate polyethyleneimine of 60000Da macromoleculars that 26.5g molecular weight is added in filtrate, after reacting 8 hours, filters, dries
Do to obtain the powdered phosphorus nitrogen synergistic water soluble polymer fire retardant of yellowish-brown, surface amino groups substitution value 50%.
Embodiment 5
(1) 10.4g neopentyl glycols and 37.2mL POCl3s are dissolved in acetonitrile first, in 85 DEG C of back flow reactions 4 hours,
Revolving, drying obtain the phosphorous chloro- 1,3,2- dioxies phosphas of intermediate 5,5- dimethyl -2- of white acyl phosphate in oneself；
(2) by the chloro- 1,3,2- dioxies phosphas of 18.5g5,5- dimethyl -2- obtained in step (1) acyl phosphoric acid in oneself after
Ester is dissolved in 1 of the potassium rhodanide containing 9.7g, in 2- dichloroethane solutions, in 60 DEG C of back flow reactions 8 hours, is filtered to remove potassium chloride,
5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
It is the nitrogenous intermediate polyethyleneimine of 600Da macromoleculars that 18g molecular weight is added in filtrate, after reacting 4 hours, filters, dries
The powdered phosphorus nitrogen synergistic water soluble polymer fire retardant of yellowish-brown, surface amino groups substitution value 50%.
Embodiment 6
(1) 10.4g neopentyl glycols and 55.8mL POCl3s are dissolved in dichloromethane first, in 85 DEG C of back flow reactions 10
Hour, revolving, drying obtain the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl phosphate in oneself；
(2) by the chloro- 1,3,2- dioxies phosphas of 18.5g5,5- dimethyl -2- obtained in step (1) acyl phosphoric acid in oneself after
Ester is dissolved in the acetone soln of the potassium rhodanide containing 9.7g, in 60 DEG C of back flow reactions 8 hours, is filtered to remove potassium chloride, is obtained 5,5- bis-
Methyl -2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate in oneself
It is the nitrogenous intermediate polyethyleneimine of 60000Da macromoleculars that 15g molecular weight is added in filtrate, after reacting 12 hours, is filtered, drying
Obtain the powdered phosphorus nitrogen synergistic water soluble polymer fire retardant of yellowish-brown, surface amino groups substitution value 90%.
Embodiment 7
Water-soluble flame retardant made from 1-6 of the embodiment of the present invention is dissolved in water, mixed with polyethers, afterwards and isocyanic acid
Ester reaction prepares polyurathamc, addition 8wt%, the limited oxygen index according to ASTM D2863-10 standard test materials
(LOI), ASTM D3801-10 standard tests UL-94 vertical combustion performances, the results are shown in Table 1.
The fire resistance test result of 1 flame-retardant expanded polyurethane of table
Claims (5)
1. a kind of preparation method of phosphorus nitrogen synergistic water soluble polymer fire retardant, the processing step and condition of this method are as follows：
(1) first by neopentyl glycol (NPG) and POCl3 (POCl3) be dissolved in solvent I, it is small in 85 DEG C of back flow reactions 4~10
When, revolving, drying obtain the phosphorous intermediate 5 of white, the dioxy phosphas of 5- dimethyl -2- chloro- 1,3,2- acyl phosphate in oneself；
(2) after by the chloro- 1,3,2- dioxies phosphas of 5,5- dimethyl -2- obtained in step (1) in oneself acyl phosphate be dissolved in and containing
In the solvent II of potassium rhodanide (KSCN), in 60 DEG C of back flow reactions 4~10 hours, be filtered to remove potassium chloride, obtain 5,5- dimethyl-
2- isothiocyano -1,3,2- dioxies phospha acyl phosphate filtrate in oneself；
(3) the 5,5- dimethyl -2- isothiocyano -1,3,2- dioxies phospha obtained again in step (2) acyl phosphate filtrate in oneself
It is middle addition the nitrogenous intermediate polyethyleneimine (PEI) of macromolecular, reaction 4~12 hours after, filter, dry yellowish-brown is powdered
Phosphorus nitrogen synergistic water soluble polymer fire retardant；
Above-mentioned chemical equation is：
(1)
(2)
The structural formula of gained phosphorus nitrogen synergistic water soluble polymer fire retardant is：
N is the positive integer more than 0 in formula.
2. preparation method according to claim 1, it is characterised in that neopentyl glycol is 1 with POCl3 molar ratio:1
~1:6, solvent I are any of dichloromethane, acetone, 1,2- dichloroethanes, acetonitrile.
3. preparation method according to claim 1, it is characterised in that the dioxy phosphas of 5,5- dimethyl -2- chloro- 1,3,2- oneself
The molar ratio of interior acyl phosphate and potassium rhodanide is 1:1, solvent II is any of acetone, 1,2- dichloroethanes.
4. preparation method according to claim 1, it is characterised in that used polyethyleneimine is branched chain type, and its is heavy
Molecular weight is 600~60000Da.
5. preparation method according to claim 1, it is characterised in that 5,5- dimethyl -2- isothiocyanos -1,3,2- dioxies
Oneself molar ratio of interior acyl phosphate and polyethyleneimine of phospha is 3:1~405:1, the substitution of polyethyleneimine surface amino groups
Spend for 50%~90%.
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Cited By (5)
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| CN114796966A (en) * | 2022-05-24 | 2022-07-29 | 重庆华航重科电气设备有限公司 | Electric cooling, arc extinguishing and fire extinguishing reagent and preparation method thereof |
| CN114874492A (en) * | 2022-04-28 | 2022-08-09 | 横店集团得邦工程塑料有限公司 | Preparation method of efficient nitrogen-phosphorus flame retardant and application of efficient nitrogen-phosphorus flame retardant in PA6 matrix |
| CN114957655A (en) * | 2022-05-18 | 2022-08-30 | 东莞市迪彩塑胶五金有限公司 | Novel phosphorus-nitrogen high-molecular flame retardant and preparation method thereof |
| CN115536912A (en) * | 2022-10-13 | 2022-12-30 | 安徽杰蓝特新材料有限公司 | Glass fiber for pipe and preparation method thereof |
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| CN114796966A (en) * | 2022-05-24 | 2022-07-29 | 重庆华航重科电气设备有限公司 | Electric cooling, arc extinguishing and fire extinguishing reagent and preparation method thereof |
| CN114796966B (en) * | 2022-05-24 | 2023-03-14 | 重庆华航重科电气设备有限公司 | Electric cooling, arc extinguishing and fire extinguishing reagent and preparation method thereof |
| CN115626985A (en) * | 2022-09-23 | 2023-01-20 | 浙大宁波理工学院 | Novel Mo-based polymer and preparation method and application thereof |
| CN115626985B (en) * | 2022-09-23 | 2023-09-05 | 浙大宁波理工学院 | Mo-based polymer and preparation method and application thereof |
| CN115536912A (en) * | 2022-10-13 | 2022-12-30 | 安徽杰蓝特新材料有限公司 | Glass fiber for pipe and preparation method thereof |
| CN115536912B (en) * | 2022-10-13 | 2023-11-21 | 安徽杰蓝特新材料有限公司 | Glass fiber for pipe and preparation method thereof |
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