CN108440749A - Flame retardant polyether polyol and preparation method thereof - Google Patents
Flame retardant polyether polyol and preparation method thereof Download PDFInfo
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- CN108440749A CN108440749A CN201810225393.4A CN201810225393A CN108440749A CN 108440749 A CN108440749 A CN 108440749A CN 201810225393 A CN201810225393 A CN 201810225393A CN 108440749 A CN108440749 A CN 108440749A
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- Prior art keywords
- flame retardant
- polyether polyol
- preparation
- retardant polyether
- melamine
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 34
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 26
- 229920000570 polyether Polymers 0.000 title claims abstract description 26
- 229920005862 polyol Polymers 0.000 title claims abstract description 25
- 150000003077 polyols Chemical class 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000004917 polyol method Methods 0.000 title description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229920000642 polymer Polymers 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 8
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 150000002924 oxiranes Chemical class 0.000 claims description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 3
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- -1 styrene compound Chemical class 0.000 claims description 3
- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical class CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 229940043237 diethanolamine Drugs 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 238000004781 supercooling Methods 0.000 claims description 2
- QPBYBLZYMNWGMO-UHFFFAOYSA-N 2,2,3-trimethyloxirane Chemical compound CC1OC1(C)C QPBYBLZYMNWGMO-UHFFFAOYSA-N 0.000 claims 1
- 238000006735 epoxidation reaction Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 239000011496 polyurethane foam Substances 0.000 description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 3
- 150000007974 melamines Chemical class 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- PQXKWPLDPFFDJP-UHFFFAOYSA-N 2,3-dimethyloxirane Chemical compound CC1OC1C PQXKWPLDPFFDJP-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013844 butane Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical class CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical group O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/70—Other substituted melamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3819—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen
- C08G18/3842—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring
- C08G18/3851—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring containing three nitrogen atoms in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5021—Polyethers having heteroatoms other than oxygen having nitrogen
- C08G18/5069—Polyethers having heteroatoms other than oxygen having nitrogen prepared from polyepoxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/321—Polymers modified by chemical after-treatment with inorganic compounds
- C08G65/327—Polymers modified by chemical after-treatment with inorganic compounds containing phosphorus
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polyethers (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of flame retardant polyether polyols and preparation method thereof, belong to organic high molecular compound technical field.The flame retardant polyether polyol, nitrogen content is 7 18wt.%, chlorinity is 10 35wt.%, hydroxyl value is 200 500KOH/g, viscosity is 2000 20000mPas, and with of low cost, good stability of the dimension, thermal coefficient is low, cohesive force is strong, the characteristic of good mechanical performance and high flame retardant etc..Meanwhile the present invention also provides preparation methods, including four steps, and it is scientific and reasonable, it is simple and practicable.
Description
Technical field
The present invention relates to a kind of flame retardant polyether polyols and preparation method thereof, belong to organic high molecular compound technology neck
Domain.
Background technology
Polyurethane material hard bubble has very outstanding heat-insulating property, is widely used in the heat preservations such as building, refrigeration, transport
Occasion.In many building fire cases, since the fire that polyurethane insulation coating causes is not rarely seen, hard polyurethane foam
Plastic flame performance is particularly important.Currently, although hard polyurethane foam improves the fire-retardant of foams by adding fire retardant
Performance, but cannot fundamentally solve the flammability of polyurethane foam.In addition, since the addition of additional fire retardant can cause to gather
Urethane foam physical performance declines, and with the delay of time, and fire retardant can occur phase separation with polyurethane matrix and lose
Effect is deteriorated so as to cause flame retardant effect.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of flame retardant polyether polyol, have it is of low cost,
The characteristic of good mechanical performance and high flame retardant.
Meanwhile the present invention also provides preparation methods, and it is scientific and reasonable, it is simple and practicable.
Flame retardant polyether polyol of the present invention, structure are shown in following formula：
Wherein, m 2-5；N is 2-5, k 2-5；Nitrogen content is 7-18wt.%, chlorinity 10-35wt.%, and hydroxyl value is
200-500KOH/g, viscosity 2000-20000mPas.
The preparation method of flame retardant polyether polyol of the present invention, includes the following steps：
1) melamine and propylene oxide in the reactor, is first added, adds basic amine, reacts 2 hours；
2) after supercooling, filtering and drying, intermediate polyhydroxy-melamine performed polymer is made；
3) it is put into reactor through polyhydroxy obtained-melamine performed polymer, adds epoxide and alkalinity is urged
Agent is reacted 2-4 hours, and phosphorus trichloride or phosphorus pentachloride is added, and keeps the temperature 2-4 hours；
4) by neutralizing with after refinement treatment, flame retardant polyether polyol is obtained.
With propylene oxide under the catalytic action of basic amine sudden reaction occurs for melamine.
In the step 1), reaction temperature is 60-120 DEG C, reaction pressure 0-2MPa.
In the step 1), the mass ratio of melamine and propylene oxide is 7-8:12-13；Basic amine quality accounts for three
The 0.2-0.5% of gross mass.
In the step 1), basic amine is monoethanolamine, diethanol amine, triethanolamine, urea, dimethylamine or dicyandiamide
One or more of.
In the step 3), epoxide 1,2- ethylene oxide, 1,2- propylene oxide, 1,2- epoxy butanes, two
One or more of methyl propylene oxide or change styrene compound.
In the step 3), the mass ratio of polyhydroxy-melamine performed polymer and epoxide is 11-12:8-9；
Basic catalyst quality accounts for the 0.2-0.5% of three's gross mass.
Polyhydroxy-melamine performed polymer continues that sudden reaction, phosphorus trichloride and reaction product occurs with epoxide
Continue that substitution reaction occurs, replaces part H atom with Cl atoms.
In the step 3), excessive phosphorus trichloride or phosphorus pentachloride is added.
In the step 3), reaction temperature is 60-200 DEG C, reaction pressure 0-2MPa, holding temperature 60-200
DEG C, heat preservation pressure 0-2MPa.
The phosphorus trichloride of addition, chlorine atom step of replacing 3) in generate polyether polyol in part hydrogen atom, realize
Better fire-retardant purpose.
In the step 3), basic catalyst is oxygen sodium oxide molybdena.
Compared with prior art, the present invention has the advantages that：
1. by introducing the ignition-proof elements such as chlorine, nitrogen into polyether polyol molecule, polyether polyol itself is set to have fire retardant
Characteristic, the influence so as to avoid additive flame retardant to foams mechanical property can better adapt to polyurethane foam
To the extensive demand of this raw material in plastics-production；
Flame retardant polyether polyol made from 2. have intensity height, good stability of the dimension, thermal coefficient is low, cohesive force is strong, goes out
The characteristics such as square rate height and permanent fire retardant；
3. preparation method provided by the present invention, scientific and reasonable, simple and practicable.
Specific implementation mode
With reference to embodiment, the present invention is described further.
Embodiment 1
400g melamines and 522.4g propylene oxide are added in the reactor, controls 100 DEG C, pressure 0.5MPa of temperature,
20ml triethylamines are added and make catalyst, react 2h.Stop reaction, lets cool to room temperature filtering, dry obtained intermediate polyhydroxy-three
Poly cyanamid performed polymer；500g polyhydroxy-melamine performed polymer 293g1,2- propylene oxide and 0.3g are added in the reactor
Sodium hydroxide, reacts 2h under 120 DEG C, pressure 0.5MPa, and addition 275g phosphorus trichlorides are kept the temperature under 120 DEG C, pressure 0.5MPa
2h, then after refinement treatment, chlorinity 12%, the flame retardant polyether polyol of hydroxyl value 247mgKOH/g is made.
Embodiment 2
300g melamines and 553g propylene oxide are added in the reactor, controls 100 DEG C of temperature, pressure 0.5MPa adds
Enter 30ml diethylamine and make catalyst, reacts 2h.Stop reaction, lets cool to room temperature filtering, dry obtained intermediate polyhydroxy-three
Poly cyanamid performed polymer；500g polyhydroxy-melamine performed polymer 102g1,2 epoxy butanes, 62.2g1,2 are added in the reactor
The sodium hydroxide of ethylene oxide and 0.3g, reacts 2h under 120 DEG C, pressure 0.5MPa, addition 275kg phosphorus trichlorides at 120 DEG C,
2h is kept the temperature under pressure 0.5MPa, then through refined post-processing, chlorinity 10% is made, and the flame retarding polyether of hydroxyl value 247mgKOH/g is polynary
Alcohol.
Embodiment 3
200g melamines and 461g propylene oxide are added in the reactor, controls 100 DEG C of temperature, pressure 0.5MPa adds
Enter 20ml triethylamines and make catalyst, reacts 2h.Stop reaction, lets cool to room temperature filtering, dry obtained intermediate polyhydroxy-three
Poly cyanamid performed polymer；500g polyhydroxy-melamine performed polymer 132g 1,2 epoxy prapanes and total weight are added in the reactor
The sum of 0.3g sodium hydroxide, react 2h under 120 DEG C, pressure 0.5MPa, addition 275g phosphorus trichlorides are at 120 DEG C, pressure
2h is kept the temperature under 0.5MPa, then through refined post-processing, chlorinity 13%, the flame retardant polyether polyol of hydroxyl value 270mgKOH/g is made.
In embodiment 1-3 products, following substance is added respectively, flame-retardant foam is made, test its performance；
Embodiment 1-3 products are tested for the property, test result is as shown in table 1, is surveyed according to GB2406-1993
Examination.
1 the performance test results of table
| Critical oxygen index (DOI) | Reaction time (s) | |
| Embodiment 1 | 27.9% | 32 |
| Embodiment 2 | 28.2% | 33 |
| Embodiment 3 | 28.4% | 35 |
| Commercial product | 25% | 60 |
Claims (9)
1. a kind of flame retardant polyether polyol, it is characterised in that：Structure is shown in figure below：
Wherein, m 2-5；N is 2-5, k 2-5；Nitrogen content is 7-18wt.%, chlorinity 10-35wt.%, hydroxyl value 200-
500KOH/g, viscosity 2000-20000mPas.
2. a kind of preparation method of flame retardant polyether polyol described in claim 1, it is characterised in that：Include the following steps：
1) melamine and propylene oxide in the reactor, is first added, adds basic amine, reacts 2 hours；
2) after supercooling, filtering and drying, intermediate polyhydroxy-melamine performed polymer is made；
3) it is put into reactor through polyhydroxy obtained-melamine performed polymer, adds epoxide and basic catalyst,
Phosphorus trichloride or phosphorus pentachloride is added in reaction 2-4 hours, keeps the temperature 2-4 hours；
4) by neutralizing with after refinement treatment, flame retardant polyether polyol is obtained.
3. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 1), reaction temperature
Degree is 60-120 DEG C, reaction pressure 0-2MPa.
4. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 1), melamine
The mass ratio of amine and propylene oxide is 7-8:12-13；Basic amine quality accounts for the 0.2-0.5% of three's gross mass.
5. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 1), basic amine
For one or more of monoethanolamine, diethanol amine, triethanolamine, urea, dimethylamine or dicyandiamide.
6. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 3), epoxidation
Conjunction object is 1,2- ethylene oxide, 1,2 epoxy prapane, 1,2- epoxy butanes, dimethyl propylene oxide or changes styrene compound
One or more of.
7. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 3), polyhydroxy-
The mass ratio of melamine performed polymer and epoxide is 11-12:8-9；Basic catalyst quality accounts for three's gross mass
0.2-0.5%.
8. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 3), reaction temperature
Degree is 60-200 DEG C, reaction pressure 0-2MPa, and holding temperature is 60-200 DEG C, heat preservation pressure 0-2MPa.
9. the preparation method of flame retardant polyether polyol according to claim 2, it is characterised in that：In step 3), alkalinity is urged
Agent is sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810225393.4A CN108440749A (en) | 2018-03-19 | 2018-03-19 | Flame retardant polyether polyol and preparation method thereof |
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| CN201810225393.4A CN108440749A (en) | 2018-03-19 | 2018-03-19 | Flame retardant polyether polyol and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111363135A (en) * | 2020-03-14 | 2020-07-03 | 浙江恒丰新材料有限公司 | A kind of preparation method and application of melamine-ethylene oxide/propylene oxide copolymer polyether polyol |
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|---|---|---|---|---|
| JPS6031528A (en) * | 1983-07-29 | 1985-02-18 | Nippon Shokubai Kagaku Kogyo Co Ltd | Production of polyether-polyol |
| CN102731768A (en) * | 2012-06-12 | 2012-10-17 | 四川金象赛瑞化工股份有限公司 | Method for preparing polyether glycol by using melamine as initiator |
| CN104877126A (en) * | 2015-06-25 | 2015-09-02 | 淄博德信联邦化学工业有限公司 | Synthetic method for high-activity flame-retardant polyether polyol |
-
2018
- 2018-03-19 CN CN201810225393.4A patent/CN108440749A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6031528A (en) * | 1983-07-29 | 1985-02-18 | Nippon Shokubai Kagaku Kogyo Co Ltd | Production of polyether-polyol |
| CN102731768A (en) * | 2012-06-12 | 2012-10-17 | 四川金象赛瑞化工股份有限公司 | Method for preparing polyether glycol by using melamine as initiator |
| CN104877126A (en) * | 2015-06-25 | 2015-09-02 | 淄博德信联邦化学工业有限公司 | Synthetic method for high-activity flame-retardant polyether polyol |
Non-Patent Citations (3)
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| 国家标准: "《塑料 用氧指数法测定燃烧行为 第2部分：室温试验》", 5 June 2009 * |
| 国家标准: "《塑料燃烧性能试验方法 氧指数法》", 1 April 1994 * |
| 陈金珠著: "《有机化学》", 31 January 2017, 北京理工大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111363135A (en) * | 2020-03-14 | 2020-07-03 | 浙江恒丰新材料有限公司 | A kind of preparation method and application of melamine-ethylene oxide/propylene oxide copolymer polyether polyol |
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