CN105038819A - Preparation method of novel silicane fire retardant - Google Patents
Preparation method of novel silicane fire retardant Download PDFInfo
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- CN105038819A CN105038819A CN201510587456.7A CN201510587456A CN105038819A CN 105038819 A CN105038819 A CN 105038819A CN 201510587456 A CN201510587456 A CN 201510587456A CN 105038819 A CN105038819 A CN 105038819A
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- silane
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- siloxanes
- phosphorus trichloride
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Abstract
The invention relates to a preparation method of novel silicane fire retardant. The method includes the following steps of firstly, dissolving siloxane in organic solvent with the siloxane as raw materials, adding a potassium hydroxide catalyst, and conducting heating reflux for 15-30 minutes after the mixture is stirred to be uniform so that sodium complex can be obtained; secondly, adding phosphorus trichloride for substitution after the phosphorus trichloride is slightly cooled, conducting reflux again for 25-40 minutes, and converting the phosphorus trichloride into phosphorus complex; thirdly, conducting filtering after cooling, cooling filtrate to -5 DEG C after the filtrate is concentrated, and generating white crystals; fourthly, flushing the white crystals obtained in the third step through methyl alcohol, placing the white crystals in a room-temperature vacuum oven to be dried for 0.6-1.5 hours, and obtaining the silicane fire retardant. Compared with the prior art, the reaction condition is gentle, the reaction temperature is moderate, the obtained finished product can be quite easily separated from a reaction system, the flame retardant property and the oxidation resistance can be effectively improved, and meanwhile the mechanics performance, the insulating performance and the heat resistance are not influenced.
Description
[technical field]
The present invention relates to technical field of flame retardant, specifically a kind of preparation method of novel silane fire retardant.
[background technology]
At present, existing silane fire retardant is in building-up process, the active reaction raw material used is P contained compound, this P contained compound has larger toxicity, in the process that synthesis is flame-retardant modified, P contained compound can endanger the healthy of operator, and this kind of preparation method's complex process, preparation cost is relatively high; In addition, the end product of this preparation method is not segregative mixture, wherein can remain by the product containing not clear composition, thus affect the final utilization performance of silane fire retardant, as the thermostability on silane fire retardant, water-absorbent, mechanical property, antioxidant property etc. cause bad impact.Therefore, if a kind of negative impact that can reduce to cause resistance toheat, antioxidant property etc. can be provided, and the preparation method of the silane fire retardant that finished product is easily separated from reaction system, will have very important significance.
[summary of the invention]
Object of the present invention is exactly the preparation method that will solve above-mentioned deficiency and provide a kind of novel silane fire retardant, not only reaction conditions is gentle, temperature of reaction is moderate, gained finished product can be separated easily from reaction system, and can effectively improve flame retardant properties and antioxidant property, simultaneously mechanics, insulation, resistance toheat are all unaffected.
Design a kind of preparation method of novel silane fire retardant for achieving the above object, comprise the following steps,
1) take siloxanes as raw material, be dissolved in by siloxanes in organic solvent, add potassium hydroxide catalyst, after stirring, reflux 15-30 minute, obtains sodium complex;
2), after slightly cold, add phosphorus trichloride and replace, then the 25-40 minute that refluxes, convert sodium complex to phosphorus complex;
3) after cooling, filter, after filtrate is concentrated, then be cooled to-5 DEG C, white crystal generates;
4) by step 3) the white crystal washed with methanol of gained, be then placed in the dry 0.6-1.5 hour of vacuum drying oven of room temperature, obtain silane fire retardant.
Wherein, the weight fraction of each component is: siloxanes 10-36 part, organic solvent 0.06-6.8 part, potassium hydroxide 5-16 part, phosphorus trichloride 0.02-1.7 part.
Described siloxanes is vinyltrimethoxy silane, vinyltriacetoxy silane, vinyl silane triisopropoxide, vinyltriethoxysilane, vinylbenzene ethyl trimethoxy silane, in 3-chloropropyl triethoxysilane, 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyltriethoxy diethoxy silane, 3-aminopropyl dimethylethoxysilane, 3-chloropropylmethyldimethoxysilane, any one in 3-r-chloropropyl trimethoxyl silane.
Described organic solvent is any one or a few in methyl alcohol, ethanol, Virahol, acetone, butanone, benzene,toluene,xylene, chlorobenzene, dichlorobenzene.
The present invention compared with the existing technology, take siloxanes as raw material, this siloxanes can be all kinds, take potassium hydroxide as catalyzer, by different ratios in the suitable solvent such as alcohols, ketone, benzene class, stirring heating is reacted, obtain sodium complex, recycling phosphorus trichloride replaces, and converts sodium complex to phosphorus complex, thus obtains silane fire retardant, this preparation method not only reaction conditions is gentle, temperature of reaction is moderate, does not have the generation of by product, and gained finished product can be separated easily from reaction system; In addition, the preparation method of silane fire retardant of the present invention, can improve flame retardant properties and antioxidant property effectively, and simultaneously mechanics, insulation, resistance toheat are all unaffected, are worthy of popularization.
[accompanying drawing explanation]
Fig. 1 is reaction principle schematic diagram of the present invention.
[embodiment]
Below in conjunction with specific embodiment, following further illustrating is done to the present invention:
The preparation method of silane fire retardant of the present invention, comprises the following steps:
1) take siloxanes as raw material, be dissolved in by siloxanes in organic solvent, add potassium hydroxide catalyst, after stirring, reflux 15-30 minute, obtains sodium complex;
2), after slightly cold, add phosphorus trichloride and replace, then the 25-40 minute that refluxes, convert sodium complex to phosphorus complex;
3) after cooling, filter, after filtrate is concentrated, then be cooled to-5 DEG C, white crystal generates;
4) by step 3) the white crystal washed with methanol of gained, be then placed in the dry 0.6-1.5 hour of vacuum drying oven of room temperature, obtain silane fire retardant.
Wherein, the weight fraction of each component is: siloxanes 10-36 part, organic solvent 0.06-6.8 part, potassium hydroxide 5-16 part, phosphorus trichloride 0.02-1.7 part.Siloxanes is any one in vinyltrimethoxy silane, vinyltriacetoxy silane, vinyl silane triisopropoxide, vinyltriethoxysilane, vinylbenzene ethyl trimethoxy silane, 3-chloropropyl triethoxysilane, in 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyltriethoxy diethoxy silane, 3-aminopropyl dimethylethoxysilane, 3-chloropropylmethyldimethoxysilane, 3-r-chloropropyl trimethoxyl silane.Organic solvent is any one or a few in methyl alcohol, ethanol, Virahol, acetone, butanone, benzene,toluene,xylene, chlorobenzene, dichlorobenzene.
Be below one of specific embodiments of the invention:
24.71g vinyltrimethoxy silane is dissolved in 267mL methyl alcohol, then adds 3.0g water and 9.35g potassium hydroxide, violent stirring; Solution become homogeneous after, reflux 20 minutes, after slightly cold, adds the 60mL methanol solution of 7.5 phosphorus trichlorides, then refluxes 30 minutes; After cooling, KCl salt is filtered out; Filtrate is concentrated into 100mL, then is cooled to-5 DEG C, after for some time, white crystal generates; The a small amount of washed with methanol of the crystal that suction filtration obtains, be then placed in dry 1 hour of the vacuum drying oven of room temperature, weigh to obtain 1.56g.
The present invention, by the restriction of above-mentioned embodiment, change, the modification done, substitutes, combines, simplifies under other any does not deviate from spirit of the present invention and principle, all should be equivalent substitute mode, is included within protection scope of the present invention.
Claims (4)
1. a preparation method for novel silane fire retardant, is characterized in that, comprises the following steps,
1) take siloxanes as raw material, be dissolved in by siloxanes in organic solvent, add potassium hydroxide catalyst, after stirring, reflux 15-30 minute, obtains sodium complex;
2), after slightly cold, add phosphorus trichloride and replace, then the 25-40 minute that refluxes, convert sodium complex to phosphorus complex;
3) after cooling, filter, after filtrate is concentrated, then be cooled to-5 DEG C, white crystal generates;
4) by step 3) the white crystal washed with methanol of gained, be then placed in the dry 0.6-1.5 hour of vacuum drying oven of room temperature, obtain silane fire retardant.
2. preparation method as claimed in claim 1, is characterized in that: the weight fraction of each component is: siloxanes 10-36 part, organic solvent 0.06-6.8 part, potassium hydroxide 5-16 part, phosphorus trichloride 0.02-1.7 part.
3. preparation method as claimed in claim 2, is characterized in that: described siloxanes is any one in vinyltrimethoxy silane, vinyltriacetoxy silane, vinyl silane triisopropoxide, vinyltriethoxysilane, vinylbenzene ethyl trimethoxy silane, 3-chloropropyl triethoxysilane, in 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyltriethoxy diethoxy silane, 3-aminopropyl dimethylethoxysilane, 3-chloropropylmethyldimethoxysilane, 3-r-chloropropyl trimethoxyl silane.
4. preparation method as claimed in claim 3, is characterized in that: described organic solvent is any one or a few in methyl alcohol, ethanol, Virahol, acetone, butanone, benzene,toluene,xylene, chlorobenzene, dichlorobenzene.
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| CN201510587456.7A CN105038819A (en) | 2015-09-16 | 2015-09-16 | Preparation method of novel silicane fire retardant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109749128A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | A kind of high temperature resistant silane crosslinker and preparation method thereof containing triphenylphosphonium chloride |
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| CN109749128A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | A kind of high temperature resistant silane crosslinker and preparation method thereof containing triphenylphosphonium chloride |
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Application publication date: 20151111 |