CN110606990A - Hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant and preparation method thereof - Google Patents
Hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
Abstract
The invention discloses a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant and a preparation method thereof. The raw materials of the flame retardant comprise tetraethoxysilane, phenyl siloxane, amino-terminated siloxane, an organic solvent, deionized water and ammonium polyphosphate. The preparation method comprises the following steps: mixing and dissolving ethyl orthosilicate, phenyl siloxane, amino-terminated siloxane and the like under the condition of nitrogen; dropwise adding deionized water into the obtained reaction system for reaction; dispersing ammonium polyphosphate in a mixed solution of an organic solvent and water, and adding the mixed solution into a system to obtain a solution; and distilling the solution under reduced pressure and drying to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant. The flame retardant prepared by the invention has the carbon residue up to 66.8 percent and excellent flame retardant property. The preparation method provided by the invention has the advantages of simple preparation process and mild reaction conditions, and is suitable for batch production.
Description
Technical Field
The invention relates to a flame retardant, in particular to a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant and a preparation method thereof.
Background
With the development of society and the improvement of living standard, the application range and the demand of high polymer materials are increasing continuously. However, most of high polymer materials such as polyethylene terephthalate (PET), polypropylene (PP), polyamide 6(PA6) and the like are easy to burn, and can generate a serious melt dripping phenomenon during burning, and drips with flames not only ignite surrounding articles to cause secondary burning, but also can cause harm to human bodies, thereby bringing potential safety hazards to people's life, lives and properties, and causing life and property loss. Therefore, the research on the high polymer material flame retardant is a hotspot of the current research, and has wide economic prospect and social benefit.
Intumescent Flame Retardants (IFR) have become one of the most promising flame retardants due to their halogen-free and low toxicity. Generally IFR systems consist of three components: an acid source, a gas source and a carbon source. During combustion, these three components react with each other to form a protective char layer in the form of a foam.
Ammonium polyphosphate (APP) is a widely used inorganic phosphorus flame retardant, can effectively inhibit smoke released during polymer combustion, accords with the trend of green, environmental protection, smoke reduction and high-efficiency flame retardance, and is low in production cost and easy to process. APP can play a dual role of an acid source and an air source in an IFR system, and is decomposed into polyphosphoric acid and ammonia gas when being heated, the polyphosphoric acid can catalyze the carbonization of polymers to form a porous carbon foam layer, heat, air and pyrolysis products are prevented from entering the surface of the material, and meanwhile, released incombustible gas can play a role of diluting oxygen. APP is a flame retardant additive, and is a hotspot of research on novel flame retardant materials.
Patent CN109181248A discloses a preparation method of ammonium polyphosphate coated carbon microsphere flame retardant, firstly silanization modification is carried out on Carbon Microspheres (CMS), APP is dissolved in hot water to obtain turbid liquid, then the APP turbid liquid is mixed with silanization modified CMS dispersion liquid to carry out reflux reaction, and the ammonium polyphosphate coated carbon microsphere flame retardant is prepared by coating APP on the silanization modified CMS. The flame retardant PET composite material prepared by the flame retardant can improve the flame retardant property of PET and reduce the deterioration of the flame retardant to the mechanical property of PET.
Patent CN106832410B discloses an inorganic silicon-containing flame retardant synergist, which is prepared by subjecting magnesium trisilicate to high activation treatment, and compounding the magnesium trisilicate serving as a flame retardant synergist with an IFR system containing acid sources such as APP. At high temperature, the magnesium trisilicate flame-retardant synergist can react with acid sources such as APP and the like to be converted into silicon phosphate substances and amorphous silicon dioxide, so that the flame retardant property of the flame-retardant object is improved.
Patent CN106832813A discloses a flame retardant PET resin composition, which can achieve good flame retardant effect by coating organic siloxane, nitrogen flame retardant and phosphorus flame retardant such as APP with inorganic substance. The composite flame retardant can enable PET to have the effects of charring during combustion and slagging after combustion, and effectively improves the flame retardance of the PET.
Therefore, at present, in the field of research on flame retardants, IFR systems containing APP still remain the main object of research. However, APP is generally poor in heat resistance and is susceptible to hydrolysis, which results in a reduction in the mechanical properties of the material and thus is gradually unable to meet the ever-increasing processing and use requirements of the market. The invention synthesizes a single-component IFR system by utilizing the ion exchange reaction of hyperbranched polysiloxane and APP, which not only can take the hyperbranched polysiloxane as a carbon source to improve the flame retardant efficiency of the flame retardant, but also can improve the thermal stability and the water resistance of the flame retardant.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant and a preparation method thereof.
In order to solve the technical problems, the invention provides a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant which is characterized by comprising the following raw materials in parts by weight:
preferably, the organic solvent a and the organic solvent B are respectively at least one of ethanol, methanol, tetrahydrofuran, acetone and toluene.
Preferably, the chemical structure of the phenyl siloxane is shown in the specificationWherein R is1Is any one of methoxy, ethoxy and hydroxyl, R2Is any one of methoxy, methyl, hydroxyl and phenyl.
Preferably, the amino-terminated siloxane has a chemical structural formula ofWherein R is3Is methoxy or ethoxy, R4Is any one of methoxy, ethoxy and methyl, R5Is aminoethyl propyl or propyl.
Preferably, the chemical structural formula of the hyperbranched polysiloxane-coated ammonium polyphosphate is as follows:
the invention also provides a preparation method of the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant, which is characterized by comprising the following steps of:
step 1): adding tetraethoxysilane, phenyl siloxane, amino-terminated siloxane and an organic solvent A into a reactor, mixing and dissolving under the condition of nitrogen, and cooling the reaction temperature to-5 ℃ after fully stirring;
step 2): dropwise adding deionized water into the reaction system obtained in the step 1), reacting for 1-3 h, raising the reaction temperature to 50-80 ℃, and reacting for 2-5 h;
step 3): dispersing ammonium polyphosphate into a mixed solution of an organic solvent B and water, adding the mixed solution into the system obtained in the step 2), heating to 80-100 ℃, and refluxing and stirring for 6-10 hours to obtain a solution;
step 4): distilling the solution obtained in the step 3) at 50-70 ℃ under reduced pressure and drying to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
Preferably, the volume of the organic solvent B and the water in the step 3) is (3-6): (1-3).
The flame retardant prepared by the invention has the carbon residue up to 66.8%, and has excellent flame retardant property. The preparation method provided by the invention has the advantages of simple preparation process and mild reaction conditions, and is suitable for batch production.
Drawings
FIG. 1 is a synthesis scheme of a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant provided by the present invention;
FIG. 2 is an XPS spectrum of a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant prepared in example 1;
fig. 3 is an SEM image of hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant prepared in example 1.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 20 parts of diphenylsilanol, 10 parts of 1, 3-aminopropyltriethoxysilane and 65 parts of ethanol into a reaction vessel in parts by mole, mixing and dissolving under the condition of nitrogen, and cooling the reaction temperature to 0 ℃ after fully stirring; slowly dripping 30 parts of deionized water into the solution, reacting for 2 hours, raising the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of ethanol and water in a volume ratio of 5:2, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and (3) decompressing the obtained solution at 50 ℃, and drying at 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant (the synthetic route is shown in figure 1).
The XPS spectrogram and the SEM spectrogram of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant are respectively shown in figures 2 and 3, the yield is 90 percent, and the carbon residue is 66.8 percent.
Example 2
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 20 parts of methyl phenyl silanediol, 5 parts of gamma-aminoethyl aminopropyl trimethoxy silane and 70 parts of acetone into a reaction container in parts by mole, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 40 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of acetone and water in a volume ratio of 5:1, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and carrying out reduced pressure treatment on the obtained solution at 55 ℃, and drying at 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 93%, and the residual carbon content is 64.4%.
Example 3
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 25 parts of diphenyldimethoxysilane, 10 parts of gamma-aminoethyl aminopropyltrimethoxysilane and 60 parts of tetrahydrofuran into a reaction vessel in parts by mole, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 35 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of tetrahydrofuran and water in a volume ratio of 2:1, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and carrying out reduced pressure treatment on the obtained solution at the temperature of 60 ℃, and drying at the temperature of 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 87%, and the residual carbon content is 63.6%.
Example 4
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 20 parts of diphenyldiethoxysilane, 10 parts of gamma-aminopropyltriethoxysilane and 65 parts of toluene into a reaction vessel in parts by mole, mixing and dissolving under the condition of nitrogen, cooling the reaction temperature to 0 ℃ after fully stirring, slowly dripping 30 parts of deionized water into the solution, reacting for 2 hours, heating the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of toluene and water in a volume ratio of 5:2, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and carrying out reduced pressure treatment on the obtained solution at the temperature of 60 ℃, and drying at the temperature of 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 89%, and the residual carbon content is 65.5%.
Example 5
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 20 parts of methyl phenyl silanediol, 10 parts of 1, 3-aminopropyltriethoxysilane and 65 parts of methanol into a reaction container in parts by mole, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 35 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of methanol and water in a volume ratio of 3:1, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and carrying out reduced pressure treatment on the obtained solution at the temperature of 60 ℃, and drying at the temperature of 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 92%, and the residual carbon content is 63.7%.
Example 6
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 25 parts of diphenyldiethoxysilane, 5 parts of 1, 3-aminopropyltriethoxysilane and 65 parts of ethanol into a reaction vessel by mole parts, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 30 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of ethanol and water in a volume ratio of 3:2, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and carrying out reduced pressure treatment on the obtained solution at 65 ℃, and drying at 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 88 percent, and the residual carbon content is 66.2 percent.
Example 7
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 20 parts of trimethyloxyphenylsilane, 5 parts of gamma-aminopropylmethyldiethoxysilane and 70 parts of toluene into a reaction vessel in parts by mole, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 40 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of toluene and water in a volume ratio of 3:1, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and carrying out reduced pressure treatment on the obtained solution at the temperature of 60 ℃, and drying at the temperature of 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 92%, and the residual carbon content is 65.3%.
Example 8
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 25 parts of methyl phenyl silanediol, 5 parts of gamma-aminopropyl methyl diethoxy silane and 65 parts of methanol into a reaction container in parts by mole, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 35 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of methanol and water in a volume ratio of 5:2, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and (3) carrying out reduced pressure treatment on the obtained solution at 70 ℃, and drying at 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 86 percent, and the residual carbon content is 62.8 percent.
Example 9
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 30 parts of diphenyl diethoxy silane, 5 parts of gamma-aminopropyl methyl diethoxy silane and 65 parts of acetone in parts by mole into a reaction vessel, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 40 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of acetone and water in a volume ratio of 6:1, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and (3) carrying out reduced pressure treatment on the obtained solution at 70 ℃, and drying at 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 89%, and the residual carbon content is 61.9%.
Example 10
A hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is prepared by the following specific steps:
adding 5 parts of ethyl orthosilicate, 30 parts of diphenyldiethoxysilane, 10 parts of gamma-aminoethyl aminopropyltrimethoxysilane and 55 parts of ethanol into a reaction vessel in parts by mole, mixing and dissolving under the condition of nitrogen, fully stirring, reducing the reaction temperature to 0 ℃, slowly dripping 30 parts of deionized water into the solution, reacting for 2 hours, increasing the reaction temperature to 50 ℃, and reacting for 2 hours; then dispersing ammonium polyphosphate into a mixed solution of ethanol and water in a volume ratio of 5:1, adding the mixed solution into the system, heating the mixed solution to 100 ℃, and refluxing and stirring for 6 hours to obtain a solution; and (3) carrying out reduced pressure treatment on the obtained solution at 70 ℃, and drying at 80 ℃ to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
The yield of the prepared hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is 92%, and the residual carbon content is 62.5%.
Claims (7)
1. The hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant is characterized in that the raw materials comprise the following components in molar fraction:
2. the method for preparing hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant of claim 1, wherein the organic solvent A and the organic solvent B are respectively at least one of ethanol, methanol, tetrahydrofuran, acetone and toluene.
3. The method of claim 1, wherein the phenylsiloxane has the chemical formulaWherein R is1Is any one of methoxy, ethoxy and hydroxyl, R2Is any one of methoxy, methyl, hydroxyl and phenyl.
4. The method of claim 1, wherein the amino-terminated siloxane has a chemical formula ofWherein R is3Is methoxy or ethoxy, R4Is any one of methoxy, ethoxy and methyl, R5Is aminoethyl propyl or propyl.
5. The method of preparing a hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant of claim 1, wherein the hyperbranched polysiloxane-coated ammonium polyphosphate has a chemical structural formula of:
6. the method for preparing the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant of any one of claims 1 to 5, which is characterized by comprising the following steps:
step 1): adding tetraethoxysilane, phenyl siloxane, amino-terminated siloxane and an organic solvent A into a reactor, mixing and dissolving under the condition of nitrogen, and cooling the reaction temperature to-5 ℃ after fully stirring;
step 2): dropwise adding deionized water into the reaction system obtained in the step 1), reacting for 1-3 h, raising the reaction temperature to 50-80 ℃, and reacting for 2-5 h;
step 3): dispersing ammonium polyphosphate into a mixed solution of an organic solvent B and water, adding the mixed solution into the system obtained in the step 2), heating to 80-100 ℃, and refluxing and stirring for 6-10 hours to obtain a solution;
step 4): distilling the solution obtained in the step 3) at 50-70 ℃ under reduced pressure and drying to obtain the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant.
7. The preparation method of the hyperbranched polysiloxane-coated ammonium polyphosphate flame retardant of claim 6, wherein the volume ratio of the organic solvent B to the water in the step 3) is (3-6): (1-3).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213712A (en) * | 2021-12-28 | 2022-03-22 | 海南红杉科创实业有限公司 | Flame retardant, preparation method and application thereof |
| CN114934386A (en) * | 2022-02-25 | 2022-08-23 | 浙江理工大学 | P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric and preparation method thereof |
| WO2022263562A1 (en) * | 2021-06-15 | 2022-12-22 | Siloxene Ag | Functionalized q-d/t-siloxane-based polymeric materials and formulations and method for preparing same |
| CN115612203A (en) * | 2022-09-22 | 2023-01-17 | 惠州市同益尖端新材料科技有限公司 | Flame-retardant high-gloss polypropylene composite material and preparation method thereof |
| CN116285340A (en) * | 2023-04-06 | 2023-06-23 | 陕西科技大学 | Cable core wrapping tape for high-temperature-resistant muscovite-based flexible cable and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140005298A1 (en) * | 2011-03-17 | 2014-01-02 | Rudolf Hensel Gmbh | Composition for an intumescent fire protection coating, fire protection coating, its use and manufacturing process for an intumescent fire protection coating |
| CN104479172A (en) * | 2014-12-05 | 2015-04-01 | 黑龙江省润特科技有限公司 | Preparation method of ammonium polyphosphate wrapped with fluorine-containing silicone oil on surface |
| CN105862392A (en) * | 2016-06-14 | 2016-08-17 | 东华大学 | Flame retardant coating adhesive and application thereof |
| CN106700920A (en) * | 2017-01-22 | 2017-05-24 | 太原理工大学 | Reaction type polysiloxane flame-retardant coating and preparation method thereof |
| CN109137467A (en) * | 2018-06-27 | 2019-01-04 | 华南理工大学 | The method that one kettle way prepares super-hydrophobic fire-retardant textile fabric |
| CN110016139A (en) * | 2019-04-01 | 2019-07-16 | 东华大学 | A kind of Containing Schiff-bases hyperbranched polyorganosiloxane fire retardant and the preparation method and application thereof |
-
2019
- 2019-09-11 CN CN201910858401.3A patent/CN110606990A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140005298A1 (en) * | 2011-03-17 | 2014-01-02 | Rudolf Hensel Gmbh | Composition for an intumescent fire protection coating, fire protection coating, its use and manufacturing process for an intumescent fire protection coating |
| CN104479172A (en) * | 2014-12-05 | 2015-04-01 | 黑龙江省润特科技有限公司 | Preparation method of ammonium polyphosphate wrapped with fluorine-containing silicone oil on surface |
| CN105862392A (en) * | 2016-06-14 | 2016-08-17 | 东华大学 | Flame retardant coating adhesive and application thereof |
| CN106700920A (en) * | 2017-01-22 | 2017-05-24 | 太原理工大学 | Reaction type polysiloxane flame-retardant coating and preparation method thereof |
| CN109137467A (en) * | 2018-06-27 | 2019-01-04 | 华南理工大学 | The method that one kettle way prepares super-hydrophobic fire-retardant textile fabric |
| CN110016139A (en) * | 2019-04-01 | 2019-07-16 | 东华大学 | A kind of Containing Schiff-bases hyperbranched polyorganosiloxane fire retardant and the preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 武翠翠等: "聚硅氧烷表面改性聚磷酸铵的制备及阻燃应用", 《塑料》 * |
| 诸健强等: "苯基聚硅氧烷微胶囊化聚磷酸铵的制备及其在PP中阻燃性能研究", 《中国塑料》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022263562A1 (en) * | 2021-06-15 | 2022-12-22 | Siloxene Ag | Functionalized q-d/t-siloxane-based polymeric materials and formulations and method for preparing same |
| CN114213712A (en) * | 2021-12-28 | 2022-03-22 | 海南红杉科创实业有限公司 | Flame retardant, preparation method and application thereof |
| CN114213712B (en) * | 2021-12-28 | 2024-02-02 | 海南红杉科创实业有限公司 | Flame retardant, preparation method and application thereof |
| CN114934386A (en) * | 2022-02-25 | 2022-08-23 | 浙江理工大学 | P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric and preparation method thereof |
| CN115612203A (en) * | 2022-09-22 | 2023-01-17 | 惠州市同益尖端新材料科技有限公司 | Flame-retardant high-gloss polypropylene composite material and preparation method thereof |
| CN116285340A (en) * | 2023-04-06 | 2023-06-23 | 陕西科技大学 | Cable core wrapping tape for high-temperature-resistant muscovite-based flexible cable and preparation method thereof |
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Application publication date: 20191224 |