CN100475932C - Preparation method of chlorobromoalkyl phosphate flame retardant - Google Patents
Preparation method of chlorobromoalkyl phosphate flame retardant Download PDFInfo
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- CN100475932C CN100475932C CNB2007100615453A CN200710061545A CN100475932C CN 100475932 C CN100475932 C CN 100475932C CN B2007100615453 A CNB2007100615453 A CN B2007100615453A CN 200710061545 A CN200710061545 A CN 200710061545A CN 100475932 C CN100475932 C CN 100475932C
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 48
- 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 21
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 17
- 239000010452 phosphate Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 22
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 19
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 10
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 8
- 238000005893 bromination reaction Methods 0.000 claims abstract description 5
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000005886 esterification reaction Methods 0.000 claims abstract description 3
- 238000007363 ring formation reaction Methods 0.000 claims abstract description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims abstract 5
- 238000006243 chemical reaction Methods 0.000 claims description 27
- -1 2,2-dibromomethyl propyl bromide diphosphoryl chloride Chemical compound 0.000 claims description 7
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 7
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- 238000006482 condensation reaction Methods 0.000 claims description 3
- 239000001294 propane Substances 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- HRBGNYVNFUBXQJ-UHFFFAOYSA-N 3,9-dichloro-3,9-diphosphaspiro[5.5]undecane-2,4,8,10-tetrone Chemical compound C1C(=O)P(Cl)C(=O)CC21CC(=O)P(Cl)C(=O)C2 HRBGNYVNFUBXQJ-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 claims 1
- 238000007142 ring opening reaction Methods 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000460 chlorine Substances 0.000 abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 5
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 230000031709 bromination Effects 0.000 abstract description 2
- 239000012190 activator Substances 0.000 abstract 1
- 150000002148 esters Chemical class 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 11
- 229910052794 bromium Inorganic materials 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 9
- 239000003112 inhibitor Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 6
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229940059574 pentaerithrityl Drugs 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 150000003014 phosphoric acid esters Chemical class 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 125000001246 bromo group Chemical group Br* 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- 241000237502 Ostreidae Species 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 235000020636 oyster Nutrition 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical class ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical class CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- 229920006305 unsaturated polyester Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- OLGLPMIHSCHZMK-UHFFFAOYSA-N BrC1(C(C(=O)O)C=CC(=C1C(=O)O)C)Br Chemical compound BrC1(C(C(=O)O)C=CC(=C1C(=O)O)C)Br OLGLPMIHSCHZMK-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- SKRKROTYQLXALL-UHFFFAOYSA-N [P]Br Chemical compound [P]Br SKRKROTYQLXALL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
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- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparing method of chlorine bromoalkane group phosphate ester flame retardant in flame retardant domain, which comprises the following steps: choosing pentaerythrite, phsophorus trichloride and liquid bromine, epichlorohydrin as raw material; choosing toluene, carbon tetrachloride and aluminium trichloride as findings; proceeding esterification reaction in toluene dissolvent with mole ratio of pentaerythrite and phsophorus trichloride at 1 : 2.5; stripping dissolvent; getting intermediate I; proceeding bromination in carbon tetrachloride dissolvent with mole ratio of intermediate I and liquid bromine at 1 : 4.2; generating intermediate II; proceeding open cyclocondensation reaction under the condition of activator with mole ratio of intermediate II and epichlorohydrin at 1 : 4.2; getting the product. This product possesses good flame-proof property for plastic and macromolecule, which is an addition type flame retardant of extensive use.
Description
Technical field:
The preparation method of a kind of organic materials fire retardant that the present invention relates to, the preparation method of chlorobromoalkyl phosphate combustion inhibitor specifically, this fire retardant is widely used in fabric fire-retardant of organic polymer material, plastics, natural and organic synthesis.
Background technology:
The fire retardant that is most widely used at present is organic halogenated flame retardant, and wherein the application quantity maximum then is the organic bromine flame retardant.The flame-retarded efficiency of bromine is generally than the high 2.5-4 of chlorine times, and this is that the H-Br bonding strength is bigger than H-Cl, so the bromine-containing compound flame retardant effect is greater than similar chlorine-containing compound because structurally.In addition, bromide fire retardant toxicity is low, the bromine carbon bond than corresponding chlorine carbon bond a little less than, be heated and easily decompose, residual few in environment, it is good also to have in addition with the superpolymer consistency, does not worsen plurality of advantages such as the physical and mechanical properties of base material and electric property.These factors make bromide fire retardant become first-selected halogen fire retardant.But the main drawback of bromide fire retardant is to reduce by the ultraviolet stability of ignition resistant substrate, generates more cigarette, corrosive gases and toxic gas during burning, and environment is had certain influence.
Organic phosphorus flame retardant also is a very important class organic fire-retardant, and there is multiple oxidation state in P contained compound.Their decomposes product has very strong dehydration, can make the polymer surfaces charing that is covered, and forms carbon membrane, plays fire retardation.In the middle of organic phosphorus flame retardant, most important fire retardant is the phosphoric acid ester fire retardant, and phosphoric acid ester and resin compatible are good, are widely used.
Halogen phosphoric acid ester fire retardant contains halogen and phosphoric simultaneously in molecule, can fire retardation take place simultaneously in gas phase and condensed phase, and flame retardant effect is strengthened because of synergy.In order to reach the good flame effect when adapting to environmental requirement, novel bromide fire retardant kind is just constantly developed in countries in the world.The new technology of at present promising improvement bromide fire retardant performance is exactly a Halogen phosphoric acid ester fire retardant.
Summary of the invention:
The purpose of this invention is to provide a kind of is raw material with phosphorus trichloride, tetramethylolmethane, liquid bromine, epoxy chloropropane, and toluene is solvent, and aluminum trichloride (anhydrous) is the preparation method that catalyzer divides three step synthetic chlorobromoalkyl phosphate combustion inhibitors.Halophosphate of the present invention contains chlorine, bromine and phosphoric simultaneously in molecule, the existence of bromine has improved the flame retardant effect in the gas phase, the existence of chlorine has overcome the stability problem of bromine to light, the existence of phosphorus has improved the flame retardant effect in the solid phase, therefore, fire retardation can take place in gas phase and condensed phase in this fire retardant simultaneously, and flame retardant effect is strengthened because of synergy, and environmental pollution is little.
The invention has the beneficial effects as follows, bring into play better flame-retarded efficiency, and can overcome some shortcomings of simple bromide fire retardant by chlorine, bromo-phosphorus synergy; The flame retarding efficiency height especially has the good flame performance to organic materialss such as plastics and polymers, is the additive flame retardant that has wide range of applications, and has advantages such as consistency is good, thermostability is high, volatility is low, low toxicity, hydrolysis; React in the 3rd step and used epoxy chloropropane, simple to operate, the safety of its preparation method as cyclization reagent.
Description of drawings
Fig. 1 is a thermogravimetric analysis experimental result picture of the present invention.
Embodiment:
The present invention will be further described below in conjunction with specific embodiment.
It is raw material that the present invention adopts tetramethylolmethane, phosphorus trichloride, liquid bromine, epoxy chloropropane, toluene, tetracol phenixin, aluminum trichloride (anhydrous), through over-churning, bromination, three step of open loop condensation building-up reactions, prepare a kind of novel chlorobromoalkyl phosphate combustion inhibitor, it has following chemical structural formula:
1. the preparation of fire retardant
Chlorobromoalkyl phosphate combustion inhibitor of the present invention can be according to following technical qualification preparation.
(1) in having the reactor of whipping appts, adds tetramethylolmethane and toluene solvant, in half an hour, be added dropwise to phosphorus trichloride into 2.5 times of molar weights of tetramethylolmethane, and temperature is raised to 50 ℃ gradually, behind the insulated and stirred reaction 1h, again temperature is elevated to 80 ℃ gradually, insulation reaction is emitted up to no HCl gas.Remove through underpressure distillation desolvate, excessive phosphorus trichloride and a spot of by product HCl gas, obtain colorless transparent viscous liquid, be cooled to room temperature, obtain the intermediate compound I of white solid, promptly 3,9-two chloro-2,4,8,10-four oxos-3,9-two phospha spiral shell [5.5] undecanes.Above-mentioned esterification formula is expressed as:
(2) intermediate compound I is placed the reactor that has whipping appts and cooling and reflux device, add carbon tetrachloride solvent and make its dissolving, dripping mol ratio is 2.1 times liquid bromine of intermediate compound I, control reaction temperature is in 45～50 ℃ of scopes, carry out bromination reaction, become orange from oyster white, obtain intermediate II up to reaction solution, promptly 2,2-dibromo methyl-propyl bromo two phosphoryl chlorides.The intermediate II that reaction generates is a solution state, can be not treated, directly enter next reaction member.
Above-mentioned bromination reaction can be expressed with following reaction formula:
(3) intermediate II is placed the reactor that has whipping appts and cooling and reflux device, with the aluminum trichloride (anhydrous) is catalyzer, under suitable temperature, drip epoxy chloropropane,, make novel bromine chloroalkyl phosphate esters fire retardant of the present invention through the open loop condensation reaction.In this step reaction, the optimum mole ratio of reaction is 1: 4.2 (intermediate II: epoxy chloropropane); Initial reaction temperature is 50 ℃, and the end reaction temperature is 65 ℃; Optimum reacting time is controlled in 3～7 hours and finishes.Above-mentioned open loop condensation reaction can be expressed with following reaction formula:
With the crude product of this fire retardant with 15% yellow soda ash alkali cleaning after, wash again until neutrality, after underpressure distillation to there not being cut, obtain yellow transparent thick liquid product chlorine bromo alkyl phosphate type fire retardant, promptly 2,2-dibromo methyl isophthalic acid, 3-two [2-bromo-3-chloropropyl-2-chloro-3-chloropropyl phosphoric acid ester] propane.
2. flame retardant performance characterizes
According to the technology of preparing of novel chlorobromoalkyl phosphate combustion inhibitor provided by the invention, to the product 2 of preparation, 2-dibromo methyl isophthalic acid, the performance of 3-two [2-bromo-3-chloropropyl-2-chloro-3-chloropropyl phosphoric acid ester] propane is measured.
(1) measuring physical properties
Adopt corresponding national standards that the acid number of product, water content, viscosity, density etc. are analyzed.The physical performance index and the analytical standard of product see the following form.
(2) mensuration of oxygen index
The synthetic fire retardant of institute is joined in the unsaturated polyester, measure its limiting oxygen index(LOI), the result is: when the fire retardant add-on was 5%, limiting oxygen index(LOI) LOI was 28.0; When adding 10%, limiting oxygen index(LOI) LOI is 29.0; When adding 15%, limiting oxygen index(LOI) LOI is 31.5.Consider that from the angle of saving cost the addition of chlorine bromo alkyl phosphate is, just can reach flame retardant effect preferably at 10% o'clock.
(3) thermogravimetric analysis
Referring to accompanying drawing 1, product has been carried out the thermogravimetric analysis experiment, by the DTG of novel chlorobromoalkyl phosphate combustion inhibitor, TG curve checking flame retardant properties.The TG curve display, in the time of 113.8 ℃, the thermal weight loss of chlorobromoalkyl phosphate combustion inhibitor does not almost have; In the time of 270 ℃, its thermal weight loss is 15%; In the time of 340 ℃, thermal weight loss is 60.1%; Main pyrolysis temperature range is 280-350 ℃.The decomposition temperature of this temperature and most polymers is suitable, has fire-retardant preferably compatibility.The DTG curve shows that product is weightless speed maximum in the time of 306.3 ℃; And at high temperature, expanding forms comparatively compact carbon layer, and the carbon residue amount is higher, has flame retardant properties preferably.
Above-mentioned multiple compound is the commercial goods as starting raw material of the present invention.
In the building-up process of the intermediate compound I of the first step, be innovation part of the present invention for the research of solvent kind, consumption and optimum synthesis condition, purpose is to improve the mass-transfer efficiency of reaction and is applicable to suitability for industrialized production; The second and the 3rd step building-up process is innovated by the present invention.
Following example further specifies the process of the novel bromine chloroalkyl phosphate esters of preparation the present invention fire retardant, but these examples are not interpreted as limitation of the present invention in all senses.
Embodiment 1: the preparation intermediate compound I
Thermometer, CaCl will be housed
2The 100ml four-hole boiling flask of drying tube, HCl absorption unit and prolong be fixed on the magnetic stirring apparatus, add the 6g tetramethylolmethane then, the toluene solvant that adds 15ml again, drip the 9.6ml phosphorus trichloride then, in half an hour, be warmed up to 50 ℃ gradually, behind the insulated and stirred reaction 1h, again temperature be elevated to 80 ℃ gradually, insulation reaction 2h emits up to no HCl gas.Remove through underpressure distillation desolvate, excessive PCl
3With a spot of by product HCl gas, obtain colorless transparent viscous liquid, be cooled to room temperature, obtain white solid, i.e. intermediate compound I, 3,9-two chloro-2,4,8,10-four oxos-3,9-two phospha spiral shell [5.5] undecanes.
Embodiment 2: the preparation of intermediate II
With the above-mentioned four-hole boiling flask that fills intermediate compound I, load onto thermometer, prolong, CaCl
2Drying tube etc. be fixed on the magnetic stirring apparatus, add the tetracol phenixin of 11ml, stir and make solid intermediate I dissolving, dropping liquid bromine then.Reaction is violent exothermic process, and initial temperature is 40 ℃, and control ground acceleration makes temperature of reaction be controlled at 45～50 ℃.Become orange up to reaction solution from oyster white, and temperature of reaction stops the dropping liquid bromine no longer because of the dropping liquid bromine rises, at 50 ℃ of following insulation reaction 1h, promptly obtain intermediate II 2 at last, 2-dibromo methyl-propyl bromo two phosphoryl chlorides.
Embodiment 3: the preparation of bromine chloroalkyl phosphate esters fire retardant
In the reaction unit of above-mentioned intermediate II, add catalyzer aluminum trichloride (anhydrous) 0.12 gram, after waiting to dissolve 10 minutes, begin to drip the epoxy chloropropane of 12.9ml, initial reaction temperature is controlled at 50 ℃, exothermic heat of reaction is violent, the control rate of addition, making temperature of reaction is below 65 ℃, after dropwising, at 65 ℃ of insulation reaction 2h, obtain light yellow viscous liquid, remove through underpressure distillation and desolvate and other lower-boiling impurities, promptly get the crude product of chlorobromoalkyl phosphate combustion inhibitor.With the crude product of above-mentioned fire retardant with 15% yellow soda ash alkali cleaning after, wash until neutrality, underpressure distillation obtains the yellow transparent thick liquid to there not being cut under certain pressure at last again, be the finished product chlorine bromo alkyl phosphate type fire retardant, the thick yield of product can reach 94.1%.This product is used for organic materialss such as flame-proof polyvinyl chloride, polystyrene, unsaturated polyester, acrylic resin, fabric, rubber, especially has very excellent flame-retardant in soft and rigid urethane foam.
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| CN108250235B (en) * | 2016-12-28 | 2020-06-23 | 辽宁奥克化学股份有限公司 | Phosphate flame retardant material and preparation method and application thereof |
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| Title |
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| 新型阻燃剂2，2-二（溴甲基）-1，3-二[（2-溴丙基-2-氯丙基）磷酸酯]丙烷的合成研究. 丁学杰，丁松宁，方岩雄，许晖，李杰.《广东化工》，第1999年第1期. 1999 * |
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