CN104945438A - Hexaphenoxy cyclotriphosphazene production technology - Google Patents
Hexaphenoxy cyclotriphosphazene production technology Download PDFInfo
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- CN104945438A CN104945438A CN201510351978.7A CN201510351978A CN104945438A CN 104945438 A CN104945438 A CN 104945438A CN 201510351978 A CN201510351978 A CN 201510351978A CN 104945438 A CN104945438 A CN 104945438A
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- chlorobenzene
- hexachlorocyclotriphosphazene
- hexaphenoxycyclotriphosphazene
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Abstract
The invention discloses a hexaphenoxy cyclotriphosphazene production technology. The hexaphenoxy cyclotriphosphazene production technology comprises the specific steps that phosphonitrilic chloride trimer is prepared, wherein phosphorus pentachloride, ammonium chloride, magnesium chloride, pyridine and chlorobenzene are input in a reaction still according to a certain ratio and are stirred and heated to 30-40 DEG C, a backflow reaction is carried out, filtering is carried out, and the phosphonitrilic chloride trimer is obtained; synthesis is carried out, wherein chlorobenzene and phenol are input in the reaction still, and are stirred and dissolved, a sodium hydroxide solution is added in the reaction still, stirring is carried out for 25-35 min, the mixture is heated to be dewatered, then tetrabutylammonium bromide is added in the completely dewatered mixture, the phosphonitrilic chloride trimer is dropwise added after the mixture is stirred and dissolved, the backflow reaction is carried out for 16-18 h, then reaction liquid is cooled to be at 70-80 DEG C, 5% alkali liquor is added, stirring is carried out for 1-2 h, and water phases are separated and removed; organic phases are repeatedly washed and dewatered, and the product hexaphenoxy cyclotriphosphazene is obtained. The hexaphenoxy cyclotriphosphazene production technology is simple and can be achieved at the moderate and low temperature environments, the production period is short, secondary products are easy to collect, the chlorobenzene solvent can be recycled, the cost is saved, and the hexaphenoxy cyclotriphosphazene production technology is environmentally friendly.
Description
Technical field
The present invention relates to modified-high polymer field of fire-proof technology, particularly relate to the production technique of hexaphenoxycyclotriphosphazene.
Background technology
Superpolymer with its cheap price, excellent performance, is used and replaces some metallic substance in actual life in various fields, but hinders widening of its Application Areas and develop due to the inflammableness of superpolymer.Show after deliberation, phosphazene compound is replaced by organic group due to the halogen atom in molecular structure, and the P-N of high-content forms collaboration system and has good flame retardant properties, has excellent modified function to polymer materials.
Summary of the invention
The object of this invention is to provide a kind of production technique following the simple but respond well hexaphenoxycyclotriphosphazene of the principles of chemistry, technique.
To achieve these goals, technical scheme of the present invention is achieved in that the production technique of hexaphenoxycyclotriphosphazene, and the concrete operation step of its production technique is as follows:
1, the preparation of hexachlorocyclotriphosphazene: in reactor according to quality than phosphorus pentachloride: ammonium chloride: magnesium chloride: agent pyridine: the ratio of chlorobenzene=580-650:15-20:6:30:1000 drops into each raw material, stirring is warming up to 30-40 DEG C, back flow reaction 9-11 hour, cross and filter excessive described ammonium chloride, magnesium chloride and byproduct, described chlorobenzene is reclaimed in the de-filter of decompression again, be cooled to 10-15 DEG C, refilter to obtain hexachlorocyclotriphosphazene;
2, the synthesis of hexaphenoxycyclotriphosphazene: drop into chlorobenzene, phenol in reactor, the sodium hydroxide solution of 30% is added after stirring and dissolving, stir 25-35 minute, heat up and remove moisture, after dehydration completely, add Tetrabutyl amonium bromide, described hexachlorocyclotriphosphazene is dripped again after stirring and dissolving, back flow reaction 16-18 hour, then cools to 70-80 DEG C by reaction solution, adds the alkali lye of 5%, stir 1-2 hour, divide phase of anhydrating; Organic phase adds the sulfuric acid of 5%, stir after 20-30 minute and divide phase of anhydrating, described organic phase adds water again and washs, stir after 50-60 minute and divide phase of anhydrating, described organic phase carries out underpressure distillation desolvation, then adds dehydrated alcohol and cools to 10-15 DEG C of crystallization, filters, dry after filter cake ethanol wash, obtain product hexaphenoxycyclotriphosphazene.
Further, it is described chlorobenzene that each component in described step 2 obtains mass ratio: phenol: sodium hydroxide: Tetrabutyl amonium bromide: hexachlorocyclotriphosphazene=75-80:50:70:4-5:30.
Further, the alkali lye of add during extracted organic phase in described step 2 described 5%, the sulfuric acid of 5%, the consumption of washing water are not less than 5 times of described hexachlorocyclotriphosphazene quality.
Further, dehydrated alcohol in described step 2: hexachlorocyclotriphosphazene is the consumption of 1:1.
The present invention has following beneficial effect: production technique of the present invention is simple, just can complete under middle low temperature environment; With short production cycle, byproduct is easily collected; Chlorobenzene solvent can be recycled, cost-saving; Environmentally friendly.
Embodiment
Embodiment 1: add the phosphorus pentachloride of 580kg, 15kg ammonium chloride, 6kg magnesium chloride, the mixing of 30kg agent pyridine in reactor, add the stirring of 1000kg chlorobenzene again and be warming up to 30 DEG C, back flow reaction 9 hours, cross and filter excessive described ammonium chloride, magnesium chloride and byproduct, described chlorobenzene is reclaimed in the de-filter of decompression again, be cooled to 10 DEG C, refilter to obtain hexachlorocyclotriphosphazene; To dropping into chlorobenzene 750kg, phenol 500kg in reactor, the sodium hydroxide solution 700kg of 30% is added after stirring and dissolving, stir 25 minutes, heat up and remove moisture, after dehydration completely, add Tetrabutyl amonium bromide 40kg, described hexachlorocyclotriphosphazene 300kg is dripped again after stirring and dissolving, back flow reaction 16 hours, then cools to 70 DEG C by reaction solution, adds the alkali lye of 5%, stir 1 hour, divide phase of anhydrating; Organic phase adds the sulfuric acid 1500kg of 5%, stir after 20 minutes and divide phase of anhydrating, described organic phase adds water 1500kg again and washs, stir after 50 minutes and divide phase of anhydrating, described organic phase carries out underpressure distillation desolvation, then adds dehydrated alcohol 300kg and cools to 10 DEG C of crystallizations, filters, dry after filter cake ethanol wash, obtain product hexaphenoxycyclotriphosphazene.
Embodiment 2: add the phosphorus pentachloride of 630kg, 17kg ammonium chloride, 6kg magnesium chloride, the mixing of 30kg agent pyridine in reactor, add the stirring of 1000kg chlorobenzene again and be warming up to 35 DEG C, back flow reaction 10 hours, cross and filter excessive described ammonium chloride, magnesium chloride and byproduct, described chlorobenzene is reclaimed in the de-filter of decompression again, be cooled to 15 DEG C, refilter to obtain hexachlorocyclotriphosphazene; To dropping into chlorobenzene 780kg, phenol 500kg in reactor, the sodium hydroxide solution 700kg of 30% is added after stirring and dissolving, stir 30 minutes, heat up and remove moisture, after dehydration completely, add Tetrabutyl amonium bromide 40kg, described hexachlorocyclotriphosphazene 300kg is dripped again after stirring and dissolving, back flow reaction 17 hours, then cools to 75 DEG C by reaction solution, adds the alkali lye of 5%, stir 1.5 hours, divide phase of anhydrating; Organic phase adds the sulfuric acid 1500kg of 5%, stir after 25 minutes and divide phase of anhydrating, described organic phase adds water 2000kg again and washs, stir after 55 minutes and divide phase of anhydrating, described organic phase carries out underpressure distillation desolvation, then adds dehydrated alcohol 300kg and cools to 15 DEG C of crystallizations, filters, dry after filter cake ethanol wash, obtain product hexaphenoxycyclotriphosphazene.
Embodiment 3: add the phosphorus pentachloride of 650kg, 20kg ammonium chloride, 6kg magnesium chloride, the mixing of 30kg agent pyridine in reactor, add the stirring of 1000kg chlorobenzene again and be warming up to 40 DEG C, back flow reaction 11 hours, cross and filter excessive described ammonium chloride, magnesium chloride and byproduct, described chlorobenzene is reclaimed in the de-filter of decompression again, be cooled to 10 DEG C, refilter to obtain hexachlorocyclotriphosphazene; To dropping into chlorobenzene 800kg, phenol 500kg in reactor, the sodium hydroxide solution 700kg of 30% is added after stirring and dissolving, stir 35 minutes, heat up and remove moisture, after dehydration completely, add Tetrabutyl amonium bromide 40kg, described hexachlorocyclotriphosphazene 300kg is dripped again after stirring and dissolving, back flow reaction 18 hours, then cools to 80 DEG C by reaction solution, adds the alkali lye of 5%, stir 2 hours, divide phase of anhydrating; Organic phase adds the sulfuric acid 1500kg of 5%, stir after 30 minutes and divide phase of anhydrating, described organic phase adds water 1800kg again and washs, stir after 60 minutes and divide phase of anhydrating, described organic phase carries out underpressure distillation desolvation, then adds dehydrated alcohol 300kg and cools to 15 DEG C of crystallizations, filters, dry after filter cake ethanol wash, obtain product hexaphenoxycyclotriphosphazene.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, other amendments that those of ordinary skill in the art make technical scheme of the present invention or equivalently to replace, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of right of the present invention.
Claims (4)
1. the production technique of hexaphenoxycyclotriphosphazene, is characterized in that, the concrete operation step of its production technique is as follows:
(1), the preparation of hexachlorocyclotriphosphazene: in reactor according to quality than phosphorus pentachloride: ammonium chloride: magnesium chloride: agent pyridine: the ratio of chlorobenzene=580-650:15-20:6:30:1000 drops into each raw material, stirring is warming up to 30-40 DEG C, back flow reaction 9-11 hour, cross and filter excessive described ammonium chloride, magnesium chloride and byproduct, described chlorobenzene is reclaimed in the de-filter of decompression again, be cooled to 10-15 DEG C, refilter to obtain hexachlorocyclotriphosphazene;
(2), the synthesis of hexaphenoxycyclotriphosphazene: drop into chlorobenzene, phenol in reactor, the sodium hydroxide solution of 30% is added after stirring and dissolving, stir 25-35 minute, heat up and remove moisture, after dehydration completely, add Tetrabutyl amonium bromide, described hexachlorocyclotriphosphazene is dripped again after stirring and dissolving, back flow reaction 16-18 hour, then cools to 70-80 DEG C by reaction solution, adds the alkali lye of 5%, stir 1-2 hour, divide phase of anhydrating; Organic phase adds the sulfuric acid of 5%, stir after 20-30 minute and divide phase of anhydrating, described organic phase adds water again and washs, stir after 50-60 minute and divide phase of anhydrating, described organic phase carries out underpressure distillation desolvation, then adds dehydrated alcohol and cools to 10-15 DEG C of crystallization, filters, dry after filter cake ethanol wash, obtain product hexaphenoxycyclotriphosphazene.
2. the production technique of hexaphenoxycyclotriphosphazene according to claim 1, it is characterized in that, it is described chlorobenzene that each component in described step (2) obtains mass ratio: phenol: sodium hydroxide: Tetrabutyl amonium bromide: hexachlorocyclotriphosphazene=75-80:50:70:4:30.
3. the production technique of hexaphenoxycyclotriphosphazene according to claim 1, it is characterized in that, the alkali lye of add during extracted organic phase in described step (2) described 5%, the sulfuric acid of 5%, the consumption of washing water are not less than 5 times of described hexachlorocyclotriphosphazene quality.
4. the production technique of hexaphenoxycyclotriphosphazene according to claim 1, is characterized in that, dehydrated alcohol in described step (2): hexachlorocyclotriphosphazene is the consumption of 1:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759947A (en) * | 2019-11-07 | 2020-02-07 | 山东省海洋化工科学研究院 | Synthesis method of hexaphenoxycyclotriphosphazene |
| CN111793092A (en) * | 2020-07-07 | 2020-10-20 | 威海金威化学工业有限责任公司 | Purification method of hexaphenoxycyclotriphosphazene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319538A (en) * | 2013-07-04 | 2013-09-25 | 南通泰通化学科技有限公司 | Preparation method of hexaphenoxy cyclotriphosphazene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103319538A (en) * | 2013-07-04 | 2013-09-25 | 南通泰通化学科技有限公司 | Preparation method of hexaphenoxy cyclotriphosphazene |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759947A (en) * | 2019-11-07 | 2020-02-07 | 山东省海洋化工科学研究院 | Synthesis method of hexaphenoxycyclotriphosphazene |
| CN111793092A (en) * | 2020-07-07 | 2020-10-20 | 威海金威化学工业有限责任公司 | Purification method of hexaphenoxycyclotriphosphazene |
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Application publication date: 20150930 |