CN104513499A - Preparation method of silicon dioxide/ammonium polyphosphate composite flame retardant - Google Patents
Preparation method of silicon dioxide/ammonium polyphosphate composite flame retardant Download PDFInfo
- Publication number
- CN104513499A CN104513499A CN201310444576.2A CN201310444576A CN104513499A CN 104513499 A CN104513499 A CN 104513499A CN 201310444576 A CN201310444576 A CN 201310444576A CN 104513499 A CN104513499 A CN 104513499A
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- CN
- China
- Prior art keywords
- ammonium polyphosphate
- preparation
- flame retardant
- silicon dioxide
- gel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000004114 Ammonium polyphosphate Substances 0.000 title claims abstract description 19
- 235000019826 ammonium polyphosphate Nutrition 0.000 title claims abstract description 19
- 229920001276 ammonium polyphosphate Polymers 0.000 title claims abstract description 19
- 239000003063 flame retardant Substances 0.000 title claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 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 abstract description 9
- 239000002131 composite material Substances 0.000 title abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 4
- 229960001866 silicon dioxide Drugs 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001879 gelation Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 239000000499 gel Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
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- Fireproofing Substances (AREA)
Abstract
The invention discloses a preparation method of a silicon dioxide/ammonium polyphosphate composite flame retardant. The preparation method comprises the following steps: adding ammonium polyphosphate into waterless ethanol, evenly stirring, dropwise adding n-ethyl silicate, adding oxalic acid, stirring to carry out reactions for 12 minutes, dropwise adding ammonia water, adding waterless ethanol after gelation; then soaking the gel into a mixed solution of hexamethyl disilazane and n-hexane for 24 hours at a temperature of 50 DEG C, drying, and then grinding the gel so as to obtain the silicon dioxide/ammonium polyphosphate composite flame retardant. The provided preparation method has the advantage of simple and convenient synthesis route. The synthesized compound has a uniform particle size, and moreover, the flame retardant property of the compound is prominently improved compared with those of silicon dioxide and ammonium polyphosphate.
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 composite flame-retardant agent.
Background technology
Ammonium polyphosphate is one of most important kind in current inorganic phosphorus flame retardant, its phosphorus content and nitrogen content are all very high, there is again N-P synergistic effect between them, thus there is good flame retardant properties, but due to himself chemical structure, also there is a lot of problem in actual applications in it, as poor water resistance, easily reunite, the bad dispersibility in polymkeric substance body, and very easily ooze out to material surface migration when high temperature, high humidity, reduce the comprehensive effectiveness especially flame retardant properties of material.
Summary of the invention
The object of the invention is to, a kind of preparation method of silicon-dioxide/ammonium polyphosphate compound fire retardant is provided, improve oxygen index, the horizontal firing grade of material, reduce heat release rate, improve the carbon yield after material combustion, improve flame retardant effect.
A preparation method for silicon-dioxide/ammonium polyphosphate compound fire retardant, it comprises the following steps:
One, ammonium polyphosphate is joined in dehydrated alcohol, stir, drip tetraethoxy, stir, add oxalic acid, stirring reaction 12h, drip ammoniacal liquor, after gel, add dehydrated alcohol;
Two, immersed by gel in hexamethyldisilazane and normal hexane mixing solutions, at 50 DEG C of temperature, insulation 24h, dry, pulverize, obtain silicon-dioxide/ammonium polyphosphate compound fire retardant; The volume ratio of described hexamethyldisilazane and normal hexane is 1:4.
The preparation method of silicon-dioxide/ammonium polyphosphate compound fire retardant provided by the invention, its beneficial effect is, simple synthetic method, quick, the compound uniform particle sizes of synthesis, and its flame retardant properties is compared with silicon-dioxide with ammonium polyphosphate, obtain obvious improvement.
Embodiment
Below in conjunction with an embodiment, the preparation method of silicon-dioxide/ammonium polyphosphate compound fire retardant provided by the invention is described in detail.
Embodiment
One, the ammonium polyphosphate of 5g is joined in 10ml dehydrated alcohol, be placed in after high-shear whipping appts fully disperses, dropwise add 10ml tetraethoxy, add the oxalic acid 2.5ml of an acidic catalyst 0.008mol/L under magnetic stirring, at 60 DEG C of temperature, be transferred to after stirring reaction 12h in beaker, drip the ammoniacal liquor 0.2ml of basic catalyst 0.05ml/L, after gel, add a certain amount of dehydrated alcohol immediately;
Two, immersed by the wet gel after aging in the hexamethyldisilazane that volume ratio is 1:4 and normal hexane mixing solutions, carry out surface modification at 50 DEG C of temperature, modification 24h, dry, pulverize, and obtains silicon-dioxide/ammonium polyphosphate compound fire retardant.
Claims (1)
1. a preparation method for silicon-dioxide/ammonium polyphosphate compound fire retardant, is characterized in that: it comprises the following steps:
One, ammonium polyphosphate is joined in dehydrated alcohol, stir, drip tetraethoxy, stir, add oxalic acid, stirring reaction 12h, drip ammoniacal liquor, after gel, add dehydrated alcohol;
Two, immersed by gel in hexamethyldisilazane and normal hexane mixing solutions, at 50 DEG C of temperature, insulation 24h, dry, pulverize, obtain silicon-dioxide/ammonium polyphosphate compound fire retardant; The volume ratio of described hexamethyldisilazane and normal hexane is 1:4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310444576.2A CN104513499A (en) | 2013-09-27 | 2013-09-27 | Preparation method of silicon dioxide/ammonium polyphosphate composite flame retardant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310444576.2A CN104513499A (en) | 2013-09-27 | 2013-09-27 | Preparation method of silicon dioxide/ammonium polyphosphate composite flame retardant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104513499A true CN104513499A (en) | 2015-04-15 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310444576.2A Pending CN104513499A (en) | 2013-09-27 | 2013-09-27 | Preparation method of silicon dioxide/ammonium polyphosphate composite flame retardant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104513499A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862971A (en) * | 2015-05-15 | 2015-08-26 | 辽东学院 | Flame-retardant coating adhesive for textile, finishing method of flame-retardant fabric with flame-retardant coating adhesive and flame-retardant fabric with flame-retardant coating adhesive |
| CN105504879A (en) * | 2016-01-19 | 2016-04-20 | 王虹 | Method for preparing core-shell type silicon dioxide coated ammonium phosphate based on reversed-phase micro-emulsion method |
| CN106674739A (en) * | 2016-12-22 | 2017-05-17 | 阜阳市三郁包装材料有限公司 | Hybridized PAN silica aerogel modified flame-retardant polypropylene foaming plate and preparation method thereof |
| CN106810761A (en) * | 2016-12-22 | 2017-06-09 | 阜阳市三郁包装材料有限公司 | Modified polypropylene flame redardant foamed board of a kind of hydridization polytetrafluoroethylene (PTFE) silica aerogel and preparation method thereof |
| CN106832570A (en) * | 2016-12-22 | 2017-06-13 | 阜阳市三郁包装材料有限公司 | Modified polypropylene flame redardant foamed board of a kind of hybridized nanometer zinc hydroxyl stannate silica aerogel and preparation method thereof |
| CN113818105A (en) * | 2021-09-10 | 2021-12-21 | 潍坊欣龙生物材料有限公司 | Preparation method of modified intumescent flame-retardant cellulose fiber |
-
2013
- 2013-09-27 CN CN201310444576.2A patent/CN104513499A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862971A (en) * | 2015-05-15 | 2015-08-26 | 辽东学院 | Flame-retardant coating adhesive for textile, finishing method of flame-retardant fabric with flame-retardant coating adhesive and flame-retardant fabric with flame-retardant coating adhesive |
| CN105504879A (en) * | 2016-01-19 | 2016-04-20 | 王虹 | Method for preparing core-shell type silicon dioxide coated ammonium phosphate based on reversed-phase micro-emulsion method |
| CN106674739A (en) * | 2016-12-22 | 2017-05-17 | 阜阳市三郁包装材料有限公司 | Hybridized PAN silica aerogel modified flame-retardant polypropylene foaming plate and preparation method thereof |
| CN106810761A (en) * | 2016-12-22 | 2017-06-09 | 阜阳市三郁包装材料有限公司 | Modified polypropylene flame redardant foamed board of a kind of hydridization polytetrafluoroethylene (PTFE) silica aerogel and preparation method thereof |
| CN106832570A (en) * | 2016-12-22 | 2017-06-13 | 阜阳市三郁包装材料有限公司 | Modified polypropylene flame redardant foamed board of a kind of hybridized nanometer zinc hydroxyl stannate silica aerogel and preparation method thereof |
| CN113818105A (en) * | 2021-09-10 | 2021-12-21 | 潍坊欣龙生物材料有限公司 | Preparation method of modified intumescent flame-retardant cellulose fiber |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150415 |
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| WD01 | Invention patent application deemed withdrawn after publication |