CN104592168A - Preparation method fire retardant tetrabromobisphenol A bis-glycidyl ether - Google Patents
Preparation method fire retardant tetrabromobisphenol A bis-glycidyl ether Download PDFInfo
- Publication number
- CN104592168A CN104592168A CN201310520506.0A CN201310520506A CN104592168A CN 104592168 A CN104592168 A CN 104592168A CN 201310520506 A CN201310520506 A CN 201310520506A CN 104592168 A CN104592168 A CN 104592168A
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- Prior art keywords
- preparation
- tetrabromobisphenol
- bis
- glycidyl ether
- fire retardant
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/27—Condensation of epihalohydrins or halohydrins with compounds containing active hydrogen atoms
- C07D301/28—Condensation of epihalohydrins or halohydrins with compounds containing active hydrogen atoms by reaction with hydroxyl radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms
- C07D303/18—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms by etherified hydroxyl radicals
- C07D303/28—Ethers with hydroxy compounds containing oxirane rings
- C07D303/30—Ethers of oxirane-containing polyhydroxy compounds in which all hydroxyl radicals are etherified with oxirane-containing hydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1515—Three-membered rings
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a preparation method fire retardant tetrabromobisphenol A bis-glycidyl ether. The preparation method comprises following steps: step 1, tetrabromobisphenol A, sodium hydroxide solution, and epoxy chloropropane are delivered into a reaction bottle, an obtained mixture is heated to 100 to 105 DEG C, and is reacted for 0.5h, and excess epoxy chloropropane is recycled via distillation; step 2, methylbenzene and sodium hydroxide solution are delivered into the reaction bottle, an obtained mixed material is subjected to reflux reaction for 3h, and is cooled to room temperature, a precipitate is removed via filtration, pH value of an obtained filtrate is adjusted to 7 to 7.5 with saturated dibasic sodium phosphate aqueous solution, and an obtained organic phase is washed with 60 to 70 DEG C hot water until no chloride ion is detected; and step 3, an organic layer methylbenzene solution is obtained via separation, and is subjected to drying, solvent methylbenzene is recycled via distillation, and an obtained product is subjected to vacuum drying at 50 DEG C so as to obtain tetrabromobisphenol A bis-glycidyl ether. The preparation method is simple, and is high in product yield and low in production cost; and obtained tetrabromobisphenol A bis-glycidyl ether possesses excellent flam resistance and ideal cost performance.
Description
Technical field
The present invention relates to a kind of preparation method of fire retardant, be specifically related to a kind of preparation method of tetrabromo-bisphenol bisglycidyl ether.
Background technology
Because 1986 find that phenyl ether bromide fire retardant is by thermogenesis strong carcinogen many bromos dibenzodioxin alkane and PBDF, so this fire-retardant agent product fails in Europe to obtain environmental mark, be even limited to use.Very valuable specific to bromide fire retardant, so other novel bromide fire retardant is all actively being found by each state.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of fire retardant tetrabromo-bisphenol bisglycidyl ether, technique is simple, and product yield is high, reduces production cost.
The preparation method of described fire retardant tetrabromo-bisphenol bisglycidyl ether, it comprises the following steps:
One, add tetrabromo-bisphenol, sodium hydroxide solution and epoxy chloropropane in reaction flask, be warming up to 100 DEG C-105 DEG C, reaction 0.5h, the epoxy chloropropane that Distillation recovery is excessive;
Two, in reaction flask, add toluene and sodium hydroxide solution, back flow reaction 3h, be cooled to room temperature and cross and filter precipitation, it is 7-7.5 that filtrate is neutralized to pH with the saturated sodium hydrogen phosphate aqueous solution, by 60 DEG C of-70 DEG C of hot water wash to organic phase without chlorion;
Three, separate organic layer toluene solution, dry, distillating recovering solvent toluene, 50 DEG C of vacuum-dryings, obtain product tetrabromo-bisphenol bisglycidyl ether.
The preparation method of fire retardant tetrabromo-bisphenol bisglycidyl ether provided by the invention, its beneficial effect is, technique is simple, and product yield is high, and production cost is low, and gained tetrabromo-bisphenol bisglycidyl ether has good flame retardant properties and desirable cost performance.
Embodiment
Below in conjunction with an embodiment, the preparation method of fire retardant tetrabromo-bisphenol bisglycidyl ether provided by the invention is described in detail.
Embodiment
One, add 15g tetrabromo-bisphenol, 0.99g sodium hydroxide solution and 32.2ml epoxy chloropropane in reaction flask, be warming up to 100 DEG C-105 DEG C, reaction 0.5h, the epoxy chloropropane that Distillation recovery is excessive;
Two, in reaction flask, add 50ml toluene and 4.05g sodium hydroxide solution, back flow reaction 3h, be cooled to room temperature and cross and filter precipitation, it is 7-7.5 that filtrate is neutralized to pH with the saturated sodium hydrogen phosphate aqueous solution, by 60 DEG C of-70 DEG C of hot water wash to organic phase without chlorion;
Three, separate organic layer toluene solution, dry, distillating recovering solvent toluene, 50 DEG C of vacuum-dryings, obtain product tetrabromo-bisphenol bisglycidyl ether.
Claims (1)
1. a preparation method for fire retardant tetrabromo-bisphenol bisglycidyl ether, is characterized in that: it comprises the following steps:
One, add tetrabromo-bisphenol, sodium hydroxide solution and epoxy chloropropane in reaction flask, be warming up to 100 DEG C-105 DEG C, reaction 0.5h, the epoxy chloropropane that Distillation recovery is excessive;
Two, in reaction flask, add toluene and sodium hydroxide solution, back flow reaction 3h, be cooled to room temperature and cross and filter precipitation, it is 7-7.5 that filtrate is neutralized to pH with the saturated sodium hydrogen phosphate aqueous solution, by 60 DEG C of-70 DEG C of hot water wash to organic phase without chlorion;
Three, separate organic layer toluene solution, dry, distillating recovering solvent toluene, 50 DEG C of vacuum-dryings, obtain product tetrabromo-bisphenol bisglycidyl ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520506.0A CN104592168A (en) | 2013-10-30 | 2013-10-30 | Preparation method fire retardant tetrabromobisphenol A bis-glycidyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520506.0A CN104592168A (en) | 2013-10-30 | 2013-10-30 | Preparation method fire retardant tetrabromobisphenol A bis-glycidyl ether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104592168A true CN104592168A (en) | 2015-05-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310520506.0A Pending CN104592168A (en) | 2013-10-30 | 2013-10-30 | Preparation method fire retardant tetrabromobisphenol A bis-glycidyl ether |
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| CN (1) | CN104592168A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968071A (en) * | 2016-05-09 | 2016-09-28 | 开美化学科技(南通)有限公司 | Method for producing tetrabromobisphenol A diglycidyl ether |
-
2013
- 2013-10-30 CN CN201310520506.0A patent/CN104592168A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968071A (en) * | 2016-05-09 | 2016-09-28 | 开美化学科技(南通)有限公司 | Method for producing tetrabromobisphenol A diglycidyl ether |
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Application publication date: 20150506 |