CN107936296A - A kind of modified hypo-aluminum orthophosphate combustion inhibitor and preparation method - Google Patents
A kind of modified hypo-aluminum orthophosphate combustion inhibitor and preparation method Download PDFInfo
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- CN107936296A CN107936296A CN201711232629.9A CN201711232629A CN107936296A CN 107936296 A CN107936296 A CN 107936296A CN 201711232629 A CN201711232629 A CN 201711232629A CN 107936296 A CN107936296 A CN 107936296A
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- aluminum orthophosphate
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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
- 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
- C08K9/04—Ingredients treated with organic substances
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The present invention relates to flame retardant area, more particularly to a kind of modified hypo-aluminum orthophosphate combustion inhibitor, it comprises the following steps：1）Hypo-aluminum orthophosphate, dispersant are added to reaction kettle, is sufficiently stirred, solution is uniformly dispersed；2）Adhesive, modifying agent are added, heating stirring fully reaction, obtains crude product；3）Crude product is washed, filters, is obtained after drying, i.e., modified hypo-aluminum orthophosphate combustion inhibitor.The problems such as modification hypo-aluminum orthophosphate prepared by the present invention can effectively improve hypo-aluminum orthophosphate poor heat resistance, poor compatibility and bad dispersibility.
Description
Technical field
The present invention relates to flame retardant area, more particularly to a kind of modified hypo-aluminum orthophosphate combustion inhibitor and preparation method.
Background technology
In recent years, the application of high molecular material is more and more extensive, in electronic apparatus, automobile, building, weaving, space flight and aviation
Deng field, there are extensive use.However, since high molecular material burning point is low, there are serious fire hazard, to solve this
Problem, it is most common method to add fire retardant in high molecular material.The fire-retardant high molecular material of traditional halogenated flame retardant exists
There are the shortcomings of smoke amount is big, gas is poisonous during burning, disabled by many countries.Therefore research and develop environmentally friendly
Efficient halogen-free flame retardants for development high performance polymer fire proofing there is very important application value.
Hypo-aluminum orthophosphate has the advantages that phosphorus content is high, decomposition temperature is high, flame retarding efficiency is high, is a to be widely used in engineering plastic
The halogen-free flame retardants of material.Hypo-aluminum orthophosphate is applied good flame retardant effect on engineering plastics, mainly with condensed phase fire retardant mechanism
Fire retardation is played, relative to other phosphorus flame retardants, hypo-aluminum orthophosphate has the features such as additive amount is few, and hygroscopicity is small.It is but secondary
Aluminum phosphate belongs to inorganic based flame retardant, and it is poor with polymer compatibility inevitably to exist, and inequality is disperseed in high molecular material
The defects of even, and due to its poor heat resistance, spontaneous combustion easily occurs in the process of engineering plastics, there are security risk.
Seldom on how to solve the report of such performance deficiency at present, therefore, the present invention is modified hypo-aluminum orthophosphate, to improve
Performance deficiency existing for hypo-aluminum orthophosphate.
The content of the invention
The present invention provided a kind of modified hypo-aluminum orthophosphate combustion inhibitor and preparation method, and it is heat-resisting that it can effectively improve hypo-aluminum orthophosphate
The problems such as poor, poor compatibility of property and bad dispersibility.
To realize above-mentioned technical purpose, it is a kind of modified hypo-aluminum orthophosphate combustion inhibitor that the present invention, which takes specific technical solution,
Each material including following parts by weight：
100 parts of hypo-aluminum orthophosphate
1-10 parts of dispersant
0.1-20 parts of adhesive
1-50 parts of modifying agent；
Wherein, adhesive select modified waxes, polyvinyl alcohol, carboxymethyl cellulose, epoxy resin, one kind in polyacrylate or
Arbitrarily mass ratio is a variety of；
Modifying agent selects melamine cyanurate, melamine, to formvlphenoxv triazine, phenylpiperazine, polyphosphoric acid
In melamine salt, six amino rings, three phosphonitrile, hexaaniline cyclotriphosphazene, cyanuric acid, 2,4- diaminourea -6- hydroxyethylamino triazines
One kind or any mass ratio it is a variety of.
As the improved technical solution of the present invention, dispersant selects neopelex, Styrene maleic acid
Acid anhydride, citric acid, hexenyl bis-stearamides, lauryl sodium sulfate, one kind in sodium tripolyphosphate or any mass ratio it is a variety of.
As the improved technical solution of the present invention, the parts by weight of adhesive select 0.5-10 parts.
As the improved technical solution of the present invention, the parts by weight of dispersant select 1-5 parts.
As the improved technical solution of the present invention, it is prepared with the following method, comprises the following steps：
Step 1: hypo-aluminum orthophosphate is added to the water, dispersant is then added, stirs, solution is uniformly dispersed；
Step 2: adding adhesive, the modifying agent of proportional quantity, 60~180 DEG C are warming up to, stirring 2~12h of reaction, obtains crude product；
Step 3: crude product is washed, filter, modified hypo-aluminum orthophosphate combustion inhibitor is obtained after drying.
As the improved technical solution of the present invention, step 2 is specifically to add the modifying agent of proportional quantity and be heated to 60-
90 DEG C, stirring, adds the adhesive with proportional quantities and 6~12h of reaction is stirred at 80-180 DEG C, obtain crude product.
As the improved technical solution of the present invention, dry temperature is 70~150 DEG C in step 3.
It it is 80-130 DEG C as temperature dry in the improved technical scheme steps three of the present invention.
As the improved technical solution of the present invention, it is additionally included in before washing and centrifugal treating, centrifuging temperature is carried out to crude product
For 30-50 DEG C.
As the improved technical solution of the present invention, a kind of mixing time of step is 0.5-2h.
The beneficial effects of the invention are as follows：
It is specific to form effective protective film to use macromolecular substances to coat hypo-aluminum orthophosphate for modifying agent, avoid in the application
Hypo-aluminum orthophosphate is directly contacted with high molecular material, and macromolecular substances can have preferable with high molecular material because of similar compatibility principle
Dispersion effect is melted, so that hypo-aluminum orthophosphate is uniformly scattered in high molecular material；
In addition, selecting adhesive, dispersant and modifier modification hypo-aluminum orthophosphate, it not only plays hypo-aluminum orthophosphate cladding and makees
With the characteristic also having because of organic matter itself plays the purpose for reducing hypo-aluminum orthophosphate spontaneous combustion on fire；It is and tight in the formula of the application
Lattice control the proportioning of each material, therefore do not interfere with the flame retardant effect of hypo-aluminum orthophosphate.
To sum up, 1, the present invention is by adding dispersant during the reaction, avoids reaction system from reuniting caking, wraps surface
Modification efficiency is covered to greatly improve；
2nd, the present invention reduces the surface polarity of fire retardant by being modified to hypo-aluminum orthophosphate, thus improve fire retardant with
The dispersiveness and compatibility of base material, improve flame retarding efficiency；
3rd, the present invention improves the heat resistance of hypo-aluminum orthophosphate, it is not easy spontaneous combustion, greatly by being modified to hypo-aluminum orthophosphate
Improve security of the hypo-aluminum orthophosphate during production and transport；
4th, preparation method of the present invention is simple for process, and reaction time is short, and yield is high, and environment friendly and pollution-free, obtained product has
Good application prospect.
Brief description of the drawings
Fig. 1 is the infared spectrum of the modification hypo-aluminum orthophosphate combustion inhibitor 1 of embodiment 1；
Fig. 2 is the thermal weight loss collection of illustrative plates of the modification hypo-aluminum orthophosphate combustion inhibitor 1 of embodiment 1.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
A kind of modified hypo-aluminum orthophosphate combustion inhibitor, includes each material of following parts by weight：
100 parts of hypo-aluminum orthophosphate
1-10 parts of dispersant, is preferably 1-5 parts；
0.1-20 parts of adhesive, is preferably 0.5-10 parts；
1-50 parts of modifying agent；
Wherein, adhesive select modified waxes, polyvinyl alcohol, carboxymethyl cellulose, epoxy resin, one kind in polyacrylate or
Arbitrarily mass ratio is a variety of；
Modifying agent selects melamine cyanurate, melamine, to formvlphenoxv triazine, phenylpiperazine, polyphosphoric acid
In melamine salt, six amino rings, three phosphonitrile, hexaaniline cyclotriphosphazene, cyanuric acid, 2,4- diaminourea -6- hydroxyethylamino triazines
One kind or any mass ratio it is a variety of；
Dispersant selects neopelex, phenylethylene-maleic anhydride, citric acid, hexenyl bis-stearamides, ten
One kind or any mass ratio in sodium dialkyl sulfate, sodium tripolyphosphate it is a variety of.
A kind of modified hypo-aluminum orthophosphate combustion inhibitor, it is prepared with the following method, comprises the following steps：
Step 1: hypo-aluminum orthophosphate is soluble in water, dispersant is then added, is stirred（Preferably 0.5-2h）, solution is disperseed
It is even；
Step 2: adding the adhesive and modifying agent of proportional quantity, heat up 60~180 DEG C, stirring 2~12h of reaction, is slightly produced
Product；For step 2 specifically to add the modifying agent of proportional quantity and being heated to 60-90 DEG C, stirring, adds the adhesive with proportional quantities
6~12h of stirring reaction, obtains crude product at 80-180 DEG C；
Step 3: crude product is washed, filters, is dry（Drying temperature elects 70-150 DEG C as, is preferably 80~130 DEG C）After obtain
Modified hypo-aluminum orthophosphate combustion inhibitor.
Further, centrifugal treating is carried out to crude product before being additionally included in washing, centrifuging temperature is 20-60 DEG C.
As the improved technical solution of the present invention, mixing time is 0.5-2h in step 1.
The present invention is made further explanation and description with reference to specific embodiment.
Embodiment 1：
In the 200L autoclaves with agitating paddle and reflux, 150L pure water and 30kg hypo-aluminum orthophosphates are added, is opened
Stirring, then add 0.5kg lauryl sodium sulfate, stirring 1 it is small when after, add 5kg melamine cyanurates, 0.3kg
Melamine and 0.178kg cyanuric acids, stirring are warming up to 80 DEG C, and 6kg polyacrylate is finally added dropwise, is warming up to after dripping
When 180 DEG C of constant temperature stirring reaction 8 is small, after reaction, solution is cooled to 40 DEG C of progress centrifugal treatings, and with pure water two
It is secondary, centrifugation obtained solid is finally placed on 130 DEG C of drying in oven, hypo-aluminum orthophosphate 1, product yield are modified up to target product
For 97.88%.Modified hypo-aluminum orthophosphate infared spectrum manufactured in the present embodiment is as shown in Figure 1, thermal weight loss collection of illustrative plates is as shown in Figure 2.
Embodiment 2：
In the 1000L enamel reaction stills with agitating paddle and reflux, 850L pure water and 125kg hypo-aluminum orthophosphates are added, is opened
Open stirring, then add 6.25kg citric acids, when stirring 2 is small after, add 62.5kg polyphosphoric acid melamine salts, stirring heating
To 90 DEG C, be eventually adding 12.5kg modified waxes, drip rear constant temperature stirring reaction 12 it is small when, after reaction, solution is cooled down
To 35 DEG C of progress centrifugal treatings, and, centrifugation obtained solid is finally placed 80 DEG C of drying in oven, to obtain the final product with pure water twice
Target product is modified hypo-aluminum orthophosphate 2, product yield 98.5%.
Embodiment 3：
In the 5L four-hole boiling flasks with agitating paddle and reflux, 3.5L pure water and 350g hypo-aluminum orthophosphates are added, opens stirring,
Then 9g neopelexes are added, when stirring 0.5 is small after, add six amino rings of 90g, three phosphonitrile, stirring is warming up to 60
DEG C, finally be added dropwise 18g epoxy resin, be warming up to after dripping 85 DEG C stirring reaction 10 it is small when, after reaction, solution is cooled down
To less than 60 DEG C progress centrifugal treatings, and with pure water twice, finally centrifugation obtained solid is placed in 120 DEG C of baking ovens and is dried
It is dry, it is modified hypo-aluminum orthophosphate 3, product yield 96.91% up to target product.
Embodiment 4：
In the 20L four-hole boiling flasks with agitating paddle and reflux, add 15L pure water and 2500g hypo-aluminum orthophosphates, unlatching are stirred
Mix, then add 25g sodium tripolyphosphates, stirring 1.5 it is small when after, add 10g phenylpiperazines and six amino rings of 15g, three phosphonitrile,
Stirring be warming up to 75 DEG C, be eventually adding 125g polyvinyl alcohol, be warming up to after dripping 105 DEG C stirring reaction 6 it is small when, reaction terminates
Afterwards, solution is cooled to 20 DEG C of progress centrifugal treatings, and, centrifugation obtained solid is finally placed 150 DEG C with pure water twice
Drying in oven, hypo-aluminum orthophosphate 4, product yield 93.76% are modified up to target product.
Embodiment 5：
In the 50L four-hole boiling flasks with agitating paddle and reflux, 45L pure water and 6kg hypo-aluminum orthophosphates are added, opens stirring,
Then 0.2kg phenylethylene-maleic anhydrides, 0.2 citric acid and 0.2 hexenyl bis-stearamides are added, stir 1 it is small when after,
0.78kg is added to be warming up to formvlphenoxv triazine and 0.12kg 2,4- diaminourea -6- hydroxyethylamino triazines, stirring
80 DEG C, be eventually adding 0.006kg carboxymethyl celluloses, be warming up to after dripping 100 DEG C stirring reaction 8 it is small when, after reaction,
Solution is cooled to 40 DEG C of progress centrifugal treatings, and, centrifugation obtained solid is finally placed 70 DEG C of baking ovens with pure water twice
Interior drying, hypo-aluminum orthophosphate 5, product yield 95.18% are modified up to target product.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
- A kind of 1. modified hypo-aluminum orthophosphate combustion inhibitor, it is characterised in that each material including following parts by weight：100 parts of hypo-aluminum orthophosphate1-10 parts of dispersant0.1-20 parts of adhesive1-50 parts of modifying agent；Wherein, adhesive select modified waxes, polyvinyl alcohol, carboxymethyl cellulose, epoxy resin, one kind in polyacrylate or Arbitrarily mass ratio is a variety of；Modifying agent selects melamine cyanurate, melamine, to formvlphenoxv triazine, phenylpiperazine, polyphosphoric acid In melamine salt, six amino rings, three phosphonitrile, hexaaniline cyclotriphosphazene, cyanuric acid, 2,4- diaminourea -6- hydroxyethylamino triazines One kind or any mass ratio it is a variety of.
- 2. a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to claim 1, it is characterised in that dispersant selects dodecyl Benzene sulfonic acid sodium salt, phenylethylene-maleic anhydride, citric acid, hexenyl bis-stearamides, lauryl sodium sulfate, tripolyphosphate One kind or any mass ratio in sodium it is a variety of.
- 3. a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to claim 1, it is characterised in that the parts by weight of adhesive are selected 0.5-10 parts.
- 4. a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to claim 1, it is characterised in that the parts by weight of dispersant are selected 1-5 parts.
- 5. the preparation method of a kind of modification hypo-aluminum orthophosphate combustion inhibitor as described in power 1-4 is any, it is characterised in that it is using such as Lower section method is prepared, and comprises the following steps：Step 1: hypo-aluminum orthophosphate is added to the water, dispersant is then added, stirs, solution is uniformly dispersed；Step 2: adding adhesive, the modifying agent of proportional quantity, 60~180 DEG C are warming up to, stirring 2~12h of reaction, is slightly produced Product；Step 3: crude product is washed, filter, modified hypo-aluminum orthophosphate combustion inhibitor is obtained after drying.
- 6. the preparation method of a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to right wants 5, it is characterised in that step 2 is specific To add the modifying agent of proportional quantity and being heated to 60-90 DEG C, stirring, adds the adhesive with proportional quantities and is stirred at 80-180 DEG C 6~12h of reaction is mixed, obtains crude product.
- 7. the preparation method of a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to right wants 5, it is characterised in that done in step 3 Dry temperature is 70~150 DEG C.
- 8. the preparation method of a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to right wants 5, it is characterised in that done in step 3 Dry temperature is 80-130 DEG C.
- 9. the preparation method of a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to right wants 5, it is characterised in that right before washing Crude product carries out centrifugal treating, and centrifuging temperature is 20-60 DEG C.
- 10. the preparation method of a kind of modified hypo-aluminum orthophosphate combustion inhibitor according to right wants 5, it is characterised in that in step 1 Mixing time is 0.5-2h.
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Cited By (7)
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| CN109627716A (en) * | 2018-11-30 | 2019-04-16 | 广东顺德优线三维科技有限公司 | Low smell halogen-free flameproof PLA/PC material and preparation method thereof for 3D printing |
| CN109749375A (en) * | 2019-01-22 | 2019-05-14 | 广东顺德同程新材料科技有限公司 | A kind of fire retardant polybutylene terephthalate material and preparation method thereof |
| CN110615936A (en) * | 2019-10-09 | 2019-12-27 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying styrene resin and preparation method thereof |
| CN112280098A (en) * | 2019-07-25 | 2021-01-29 | 珠海万通化工有限公司 | Halogen-free flame retardant composition and two applications |
| CN113308024A (en) * | 2021-05-27 | 2021-08-27 | 武汉工程大学 | Aluminum hypophosphite-polyphosphazene core-shell type flame retardant and preparation method thereof |
| CN113321850A (en) * | 2021-06-21 | 2021-08-31 | 山东泰星新材料股份有限公司 | Ethylene-vinyl acetate halogen-free flame retardant and preparation method thereof |
| CN115322441A (en) * | 2022-09-09 | 2022-11-11 | 江西福尔鑫医药化工有限公司 | Method for producing aluminum hypophosphite flame retardant by using sodium hypophosphite mother solution |
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| CN109627716A (en) * | 2018-11-30 | 2019-04-16 | 广东顺德优线三维科技有限公司 | Low smell halogen-free flameproof PLA/PC material and preparation method thereof for 3D printing |
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| CN110615936A (en) * | 2019-10-09 | 2019-12-27 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying styrene resin and preparation method thereof |
| CN110615936B (en) * | 2019-10-09 | 2022-12-27 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying styrene resin and preparation method thereof |
| CN113308024A (en) * | 2021-05-27 | 2021-08-27 | 武汉工程大学 | Aluminum hypophosphite-polyphosphazene core-shell type flame retardant and preparation method thereof |
| CN113321850A (en) * | 2021-06-21 | 2021-08-31 | 山东泰星新材料股份有限公司 | Ethylene-vinyl acetate halogen-free flame retardant and preparation method thereof |
| CN115322441A (en) * | 2022-09-09 | 2022-11-11 | 江西福尔鑫医药化工有限公司 | Method for producing aluminum hypophosphite flame retardant by using sodium hypophosphite mother solution |
| CN115322441B (en) * | 2022-09-09 | 2024-04-05 | 江西福尔鑫医药化工有限公司 | Method for producing aluminum hypophosphite flame retardant by utilizing sodium hypophosphite mother liquor |
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Application publication date: 20180420 |
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