CN112430417A - Preparation method of ammonium polyphosphate microspheres - Google Patents
Preparation method of ammonium polyphosphate microspheres Download PDFInfo
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- CN112430417A CN112430417A CN202011310252.6A CN202011310252A CN112430417A CN 112430417 A CN112430417 A CN 112430417A CN 202011310252 A CN202011310252 A CN 202011310252A CN 112430417 A CN112430417 A CN 112430417A
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- ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention relates to the field of multifunctional modification of halogen-free flame retardants, mainly utilizes an inverse emulsion polymerization mode to coat APP to prepare ammonium polyphosphate flame-retardant microspheres, and particularly relates to a preparation method of ammonium polyphosphate microspheres. The ammonium phosphate microspheres prepared by the method can be used for thermosetting resin systems, the addition amount of the ammonium phosphate microspheres needs 15 percent, and the grade of UL94-V0 can be achieved. The residual carbon content of the epoxy resin at 700 ℃ can be greatly improved, and simultaneously, after combustion, the generated carbon layer has high strength and good barrier property, so that the flame retardance of the composite material is improved. The ammonium phosphate microspheres also reduce the negative influence of the filler on the mechanical property of the composite material.
Description
Technical Field
The invention relates to the field of multifunctional modification of a halogen-free flame retardant, and mainly relates to an ammonium polyphosphate flame-retardant microsphere prepared by coating APP in an inverse emulsion polymerization manner, belonging to the field of multifunctional modification of halogen-free flame retardants.
Background
The novel halogen-free intumescent phosphorus flame retardant is a green and environment-friendly flame retardant and is widely used for flame retardant modification of epoxy resin. However, the intumescent flame retardant has the defects of poor thermal stability, low flame retardant efficiency and large addition amount for achieving an ideal flame retardant effect, so that the mechanical property of the material is seriously damaged, and one of the ways for solving the problem is to add the synergistic flame retardant. An ideal synergistic flame retardant not only can reduce the dosage of the intumescent flame retardant, but also can improve the flame retardant property of the system. Ammonium polyphosphate (APP) is used as a phosphorus-nitrogen-containing organic flame retardant, has the functions of thermal expansion (carbonization), air isolation and heat insulation (reduction of ignition point), can promote the dehydration of a carbon layer and generate non-combustible gas by thermal decomposition, and is often used as an acid source and an air source in an expansion flame retardant system. The action mechanism is a gas-phase flame retardant mechanism, but APP and a film-forming polymer have poor compatibility and migration resistance and are easy to exude, so that the mechanical property of the steel structure fireproof coating is poor, and the application of the APP flame retardant is influenced.
To solve the above problem, we have microencapsulated our APP. At present, materials for coating APP mainly comprise melamine formaldehyde resin, polyurethane, epoxy resin and other chemical materials. However, the method of coating APP by inverse emulsion polymerization to prepare ammonium polyphosphate flame-retardant microspheres and adding the ammonium polyphosphate flame-retardant microspheres as a flame retardant to a polymer to prepare a fire-retardant coating needs further research, and therefore, a method for preparing ammonium polyphosphate microspheres is provided.
Disclosure of Invention
The invention aims to provide a preparation method of ammonium polyphosphate microspheres, which aims to solve the problems that APP and a film-forming polymer are poor in compatibility and migration resistance and easy to exude, so that a steel structure fireproof coating is poor in mechanical property, and the application of an APP flame retardant is influenced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of ammonium polyphosphate microspheres, which is characterized in that APP is coated in an inverse emulsion polymerization manner to prepare the ammonium polyphosphate flame-retardant microspheres, comprises the following steps:
s1, degrading ammonium polyphosphate by hydrogen peroxide with the mass fraction of 6% for 4-5h at the temperature of 50-70 ℃, and dialyzing for 5-10d to obtain suspension;
s2, adjusting the pH of the suspension obtained in the step S1 by using a NaOH solution with the mass fraction of 1% so that the pH is 7;
s3, rotationally evaporating the solution obtained in the step S2 to dryness, then washing with ethanol, and drying for later use;
s4, dissolving a certain amount of ground degraded carrageenan in distilled water under the water bath condition of 93-98 ℃, and dropwise adding 1% NaOH solution into the solution;
s5, preparing the solution obtained in the step S4 and the solution obtained in the step S3 into a mixture with the mass ratio of 3: 1, uniformly stirring the APP aqueous solution to serve as a water phase;
s6, weighing a certain amount of cyclohexane/chloroform, adding a certain amount of carrageenan, and uniformly stirring to obtain an oil phase;
s7: emulsifying the water phase obtained in the step S5 and the organic phase obtained in the step S6 for 10min by using a high-speed shearing emulsifying machine;
s7, transferring the emulsion into a three-necked bottle, adding epoxy chloropropane, reacting for 4 hours under the condition of water bath at the temperature of 20-30 ℃, rotationally evaporating the solvent to dryness, and centrifugally washing for 3 times by using absolute ethyl alcohol to finally prepare the ammonium polyphosphate microspheres.
Further, the washing with ethanol is performed 3 times in the step S3.
Further, cyclohexane/chloroform (volume ratio of 4: 1) in the step S6.
Further, the volume of the carrageenan in the step S6 is 1.8% -2.4% of the sum of the volumes of the cyclohexane and the chloroform.
Compared with the prior art, the invention has the beneficial effects that: the ammonium phosphate microspheres prepared by the method can be used for thermosetting resin systems, the addition amount of the ammonium phosphate microspheres needs 15 percent, and the grade of UL94-V0 can be achieved. The residual carbon content of the epoxy resin at 700 ℃ can be greatly improved, and simultaneously, after combustion, the generated carbon layer has high strength and good barrier property, so that the flame retardance of the composite material is improved. The ammonium phosphate microspheres also reduce the negative influence of the filler on the mechanical property of the composite material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described with reference to the following examples:
example 1
A preparation method of ammonium polyphosphate microspheres, which is characterized in that APP is coated in an inverse emulsion polymerization manner to prepare the ammonium polyphosphate flame-retardant microspheres, comprises the following steps:
s1, degrading ammonium polyphosphate by hydrogen peroxide with the mass fraction of 6% for 4 hours at 50 ℃, and dialyzing for 5 days to obtain suspension;
s2, adjusting the pH of the suspension obtained in the step S1 by using a NaOH solution with the mass fraction of 1% so that the pH is 7;
s3, rotationally evaporating the solution obtained in the step S2 to dryness, then washing with ethanol, and drying for later use;
s4, dissolving a certain amount of ground degraded carrageenan in distilled water under the condition of a water bath at 93 ℃, and dropwise adding a 1% NaOH solution into the solution;
s5, preparing the solution obtained in the step S4 and the solution obtained in the step S3 into a mixture with the mass ratio of 3: 1, uniformly stirring the APP aqueous solution to serve as a water phase;
s6, weighing a certain amount of cyclohexane/chloroform, adding a certain amount of carrageenan, and uniformly stirring to obtain an oil phase;
s7: emulsifying the water phase obtained in the step S5 and the organic phase obtained in the step S6 for 10min by using a high-speed shearing emulsifying machine;
and S7, transferring the emulsion into a three-necked bottle, adding epoxy chloropropane, reacting for 4 hours under the condition of water bath at the temperature of 20 ℃, rotationally evaporating the solvent to dryness, and centrifugally washing for 3 times by using absolute ethyl alcohol to finally obtain the ammonium polyphosphate microspheres.
Preferably, the washing with ethanol in the step S3 is performed 3 times.
Preferably, the volume ratio of cyclohexane/chloroform in the step S6 is 4: 1.
Preferably, the volume of the carrageenan in the step S6 is 1.8% of the sum of the volumes of the cyclohexane and the chloroform.
Example 2
A preparation method of ammonium polyphosphate microspheres, which is characterized in that APP is coated in an inverse emulsion polymerization manner to prepare the ammonium polyphosphate flame-retardant microspheres, comprises the following steps:
s1, degrading ammonium polyphosphate by hydrogen peroxide with the mass fraction of 6% for 4 hours at the temperature of 60 ℃, and dialyzing for 7d to obtain suspension;
s2, adjusting the pH of the suspension obtained in the step S1 by using a NaOH solution with the mass fraction of 1% so that the pH is 7;
s3, rotationally evaporating the solution obtained in the step S2 to dryness, then washing with ethanol, and drying for later use;
s4, dissolving a certain amount of ground degraded carrageenan in distilled water under the condition of water bath at 95 ℃, and dropwise adding 1% NaOH solution into the solution;
s5, preparing the solution obtained in the step S4 and the solution obtained in the step S3 into a mixture with the mass ratio of 3: 1, uniformly stirring the APP aqueous solution to serve as a water phase;
s6, weighing a certain amount of cyclohexane/chloroform, adding a certain amount of carrageenan, and uniformly stirring to obtain an oil phase;
s7: emulsifying the water phase obtained in the step S5 and the organic phase obtained in the step S6 for 10min by using a high-speed shearing emulsifying machine;
and S7, transferring the emulsion into a three-necked bottle, adding epoxy chloropropane, reacting for 4 hours under the condition of water bath at 25 ℃, rotationally evaporating the solvent to dryness, and centrifugally washing for 3 times by using absolute ethyl alcohol to finally obtain the ammonium polyphosphate microspheres.
Preferably, the washing with ethanol in the step S3 is performed 3 times.
Preferably, the volume ratio of cyclohexane/chloroform in the step S6 is 4: 1.
Preferably, the volume of the carrageenan in the step S6 is 2% of the sum of the volumes of the cyclohexane and the chloroform.
Example 3
A preparation method of ammonium polyphosphate microspheres, which is characterized in that APP is coated in an inverse emulsion polymerization manner to prepare the ammonium polyphosphate flame-retardant microspheres, comprises the following steps:
s1, degrading ammonium polyphosphate by hydrogen peroxide with the mass fraction of 6% for 5 hours at 70 ℃, and dialyzing for 10 days to obtain suspension;
s2, adjusting the pH of the suspension obtained in the step S1 by using a NaOH solution with the mass fraction of 1% so that the pH is 7;
s3, rotationally evaporating the solution obtained in the step S2 to dryness, then washing with ethanol, and drying for later use;
s4, dissolving a certain amount of ground degraded carrageenan in distilled water under the condition of water bath at the temperature of 98 ℃, and dropwise adding 1% NaOH solution into the solution;
s5, preparing the solution obtained in the step S4 and the solution obtained in the step S3 into a mixture with the mass ratio of 3: 1, uniformly stirring the APP aqueous solution to serve as a water phase;
s6, weighing a certain amount of cyclohexane/chloroform, adding a certain amount of carrageenan, and uniformly stirring to obtain an oil phase;
s7: emulsifying the water phase obtained in the step S5 and the organic phase obtained in the step S6 for 10min by using a high-speed shearing emulsifying machine;
and S7, transferring the emulsion into a three-necked bottle, adding epoxy chloropropane, reacting for 4 hours under the condition of water bath at the temperature of 30 ℃, rotationally evaporating the solvent to dryness, and centrifugally washing for 3 times by using absolute ethyl alcohol to finally obtain the ammonium polyphosphate microspheres.
Preferably, the washing with ethanol in the step S3 is performed 3 times.
Preferably, the volume ratio of cyclohexane/chloroform in the step S6 is 4: 1.
Preferably, the volume of the carrageenan in the step S6 is 2.4% of the sum of the volumes of the cyclohexane and the chloroform.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A preparation method of ammonium polyphosphate microspheres is characterized by comprising the following steps: coating APP by using an inverse emulsion polymerization mode to prepare the ammonium polyphosphate flame-retardant microsphere, comprising the following steps of:
s1, degrading ammonium polyphosphate by hydrogen peroxide with the mass fraction of 6% for 4-5h at the temperature of 50-70 ℃, and dialyzing for 5-10d to obtain suspension;
s2, adjusting the pH of the suspension obtained in the step S1 by using a NaOH solution with the mass fraction of 1% so that the pH is 7;
s3, rotationally evaporating the solution obtained in the step S2 to dryness, then washing with ethanol, and drying for later use;
s4, dissolving a certain amount of ground degraded carrageenan in distilled water under the water bath condition of 93-98 ℃, and dropwise adding 1% NaOH solution into the solution;
s5, preparing the solution obtained in the step S4 and the solution obtained in the step S3 into a mixture with the mass ratio of 3: 1, uniformly stirring the APP aqueous solution to serve as a water phase;
s6, weighing a certain amount of cyclohexane/chloroform, adding a certain amount of carrageenan, and uniformly stirring to obtain an oil phase;
s7: emulsifying the water phase obtained in the step S5 and the organic phase obtained in the step S6 for 10min by using a high-speed shearing emulsifying machine;
s7, transferring the emulsion into a three-necked bottle, adding epoxy chloropropane, reacting for 4 hours under the condition of water bath at the temperature of 20-30 ℃, rotationally evaporating the solvent to dryness, and centrifugally washing for 3 times by using absolute ethyl alcohol to finally prepare the ammonium polyphosphate microspheres.
2. The method for preparing ammonium polyphosphate microspheres according to claim 1, wherein the ammonium polyphosphate microspheres comprise: the washing with ethanol was performed 3 times in the step S3.
3. The method for preparing ammonium polyphosphate microspheres according to claim 1, wherein the ammonium polyphosphate microspheres comprise: the volume ratio of cyclohexane/chloroform in the step S6 is 4: 1.
4. The method for preparing ammonium polyphosphate microspheres according to claim 1, wherein the ammonium polyphosphate microspheres comprise: the volume of the carrageenan in the step S6 is 1.8-2.4% of the sum of the volumes of the cyclohexane and the chloroform.
5. The method for preparing ammonium polyphosphate microspheres according to claim 1, wherein the ammonium polyphosphate microspheres comprise: a preparation method of ammonium polyphosphate microspheres comprises the following steps;
s1, degrading ammonium polyphosphate by hydrogen peroxide with the mass fraction of 6% for 4 hours at the temperature of 60 ℃, and dialyzing for 7d to obtain suspension;
s2, adjusting the pH of the suspension obtained in the step S1 by using a NaOH solution with the mass fraction of 1% so that the pH is 7;
s3, rotationally evaporating the solution obtained in the step S2 to dryness, then washing with ethanol, and drying for later use;
s4, dissolving a certain amount of ground degraded carrageenan in distilled water under the condition of water bath at 95 ℃, and dropwise adding 1% NaOH solution into the solution;
s5, preparing the solution obtained in the step S4 and the solution obtained in the step S3 into a mixture with the mass ratio of 3: 1, uniformly stirring the APP aqueous solution to serve as a water phase;
s6, weighing a certain amount of cyclohexane/chloroform, adding a certain amount of carrageenan, and uniformly stirring to obtain an oil phase;
s7: emulsifying the water phase obtained in the step S5 and the organic phase obtained in the step S6 for 10min by using a high-speed shearing emulsifying machine;
and S7, transferring the emulsion into a three-necked bottle, adding epoxy chloropropane, reacting for 4 hours under the condition of water bath at 25 ℃, rotationally evaporating the solvent to dryness, and centrifugally washing for 3 times by using absolute ethyl alcohol to finally obtain the ammonium polyphosphate microspheres.
6. The method for preparing ammonium polyphosphate microspheres according to claim 5, wherein the ammonium polyphosphate microspheres comprise: the washing with ethanol was performed 3 times in the step S3.
7. The method for preparing ammonium polyphosphate microspheres according to claim 5, wherein the ammonium polyphosphate microspheres comprise: the volume ratio of cyclohexane/chloroform in the step S6 is 4: 1.
8. The method for preparing ammonium polyphosphate microspheres according to claim 1, wherein the ammonium polyphosphate microspheres comprise: the volume of the carrageenan in the step S6 is 2% of the sum of the volumes of the cyclohexane and the chloroform.
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| CN202011310252.6A CN112430417A (en) | 2020-11-20 | 2020-11-20 | Preparation method of ammonium polyphosphate microspheres |
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|---|---|---|---|---|
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2020
- 2020-11-20 CN CN202011310252.6A patent/CN112430417A/en active Pending
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| KR20160005672A (en) * | 2012-07-18 | 2016-01-15 | 신현우 | The composition of cosmetic patch and cosmetic pack having two -component type |
| 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 |
| CN105820609A (en) * | 2016-04-15 | 2016-08-03 | 安徽开林新材料股份有限公司 | Heat-resistant aluminum electrode anticorrosive coating and preparation method thereof |
| CN105885615A (en) * | 2016-05-16 | 2016-08-24 | 李军 | Building external wall fireproof coating and preparation method |
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Application publication date: 20210302 |