CN115109316A - Whiteness red phosphorus fire retardant and preparation method thereof - Google Patents
Whiteness red phosphorus fire retardant and preparation method thereof Download PDFInfo
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- CN115109316A CN115109316A CN202210796183.7A CN202210796183A CN115109316A CN 115109316 A CN115109316 A CN 115109316A CN 202210796183 A CN202210796183 A CN 202210796183A CN 115109316 A CN115109316 A CN 115109316A
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- red phosphorus
- flame retardant
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- zinc
- phosphorus flame
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000003063 flame retardant Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 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 claims abstract description 44
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims abstract description 27
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011701 zinc Substances 0.000 claims abstract description 25
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002775 capsule Substances 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 12
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000003751 zinc Chemical class 0.000 claims abstract description 10
- 239000011787 zinc oxide Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims 2
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 238000003756 stirring Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000002861 polymer material Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229920000877 Melamine resin Polymers 0.000 description 4
- 239000004640 Melamine resin Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- -1 zeolite imidazole ester Chemical class 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
-
- 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
- C08K3/02—Elements
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34928—Salts
-
- 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
- C08K3/02—Elements
- C08K2003/026—Phosphorus
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention provides a preparation method of a whiteness red phosphorus flame retardant, which comprises the following steps: (1) dispersing red phosphorus and a dispersing agent in water, adding cyanuric acid and zinc oxide, and reacting for 2-6 h; (2) adding soluble zinc salt and 2-methylimidazole, reacting for 6-30 h, and dehydrating and drying the precipitate to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials. The whiteness red phosphorus flame retardant provided by the invention has the characteristics of high whiteness, good oxidation resistance and high flame retardant efficiency.
Description
Technical Field
The invention relates to the field of flame retardant materials, and particularly relates to a whiteness red phosphorus flame retardant and a preparation method thereof.
Background
Compared with other halogen-free flame retardants, the red phosphorus flame retardant has the advantages of high flame retardant efficiency, small using amount and the like, and is widely applied to the fields of rubber, nylon, polyester, epoxy resin, polyurethane and the like. However, pure red phosphorus has the defects of easy moisture absorption, unstable property, poor compatibility with high polymer materials, easy coloring and the like. After the red phosphorus is coated, the stability is improved, and the compatibility with a high polymer material is better. In addition, after the purple red of the red phosphorus is covered by the capsule material, the prepared whiteness red phosphorus has relatively light color and can be used for processing light-color high polymer material products. Therefore, the whiteness red phosphorus serving as a flame retardant is added into a high polymer material, so that the defect of direct use of the red phosphorus can be overcome, and a considerable or even better flame retardant effect can be achieved.
At present, the mature red phosphorus coated product in the market is melamine resin coated red phosphorus, which takes melamine resin as a capsule wall material, has the characteristics of good oxidation resistance, low moisture absorption rate and good compatibility with high polymer materials, and is widely applied to processing of nylon, PET, PP and the like (pandeming, university of China and south, doctor thesis, 2004). However, melamine resin is transparent polymer resin, has poor covering property on red phosphorus color, has dark color, and cannot be used for processing light-colored polymer material products. In addition, the patent reports that the red phosphorus flame retardant coated by the zeolite imidazole ester framework material and the preparation method (CN 202011228743.6) thereof, and the ZIF-8 can be uniformly coated on the surface of the red phosphorus, so that the prepared ZIF-8 coated red phosphorus has better whiteness, oxidation resistance and flame retardant property. However, compared with common inorganic coating materials such as melamine resin, aluminum hydroxide and the like, the raw material cost of the ZIF-8 is high, and the large-scale application of the ZIF-8 coated red phosphorus is influenced. Therefore, the red phosphorus is compositely coated by the ZIF-8 and the cheap material, so that the production cost is reduced, the whiteness and the flame retardant property of the whiteness red phosphorus flame retardant are further improved, and the method still has important significance for expanding the application range of the red phosphorus flame retardant.
Disclosure of Invention
The invention aims to provide a preparation method of a whiteness red phosphorus flame retardant, and the whiteness red phosphorus flame retardant obtained by the method has the advantages of high whiteness, good oxidation resistance, high flame retardant efficiency, lower cost and the like.
The invention provides a preparation method of a whiteness red phosphorus flame retardant, which comprises the following steps:
(1) dispersing red phosphorus and a dispersing agent in water, adding cyanuric acid and zinc oxide, and reacting for 2-6 h;
(2) adding soluble zinc salt and 2-methylimidazole, reacting for 6-30 h, and dehydrating and drying the precipitate to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials.
Further, the dispersing agent is sodium dodecyl benzene sulfonate, sodium dodecyl sulfate or polyvinylpyrrolidone, and the mass ratio of the dispersing agent to red phosphorus is 0.5-3: 100.
further, the reaction temperature is 70-100 ℃.
Further, the molar ratio of cyanuric acid to red phosphorus is 0.2-0.4: 1.
further, the molar ratio of the cyanuric acid to the zinc oxide is 2-2.3: 3.
further, the zinc salt is zinc acetate, zinc nitrate, zinc chloride or zinc sulfate.
Further, Zn is contained in the zinc salt 2+ The molar ratio of the red phosphorus to the red phosphorus is 0.1-0.2: 1.
further, Zn is contained in the zinc salt 2+ The molar ratio to 2-methylimidazole is 1: 3 to 9.
The invention also provides a whiteness red phosphorus flame retardant, which is prepared from red phosphorus, cyanuric acid, zinc oxide, zinc salt and 2-methylimidazole through a self-assembly method and is characterized in that the red phosphorus is compositely coated with zinc cyanurate and ZIF-8.
The preparation method provided by the invention has the advantages that the process is simple, the red phosphorus surface is coated with zinc cyanurate, and then a ZIF-8 shell layer is self-assembled on the outer layer of the red phosphorus surface, the coating is uniform, the red phosphorus surface has better color covering performance, and the prepared whiteness red phosphorus flame retardant has the characteristics of high whiteness and good oxidation resistance, so that the red phosphorus flame retardant can be applied to processing of light-colored high polymer materials.
The zinc cyanurate is a flame retardant with good color covering property and low cost; ZIF-8 is a novel capsule wall material which can be continuously self-assembled on the surface of a solid, can be uniformly coated on the surface of the solid, and has better synergistic flame retardant property. The zinc cyanurate and the ZIF-8 are used as the composite capsule wall material of the whiteness red phosphorus, and the advantages of the zinc cyanurate and the ZIF-8 can be effectively combined, so that the whiteness and the flame retardant property of the prepared zinc cyanurate and ZIF-8 composite coated red phosphorus are superior to those of zinc cyanurate or ZIF-8 single coated red phosphorus. Zinc cyanurate and ZIF-8 are used as the composite capsule wall material for coating red phosphorus, and have good synergistic effect.
Detailed Description
The following provides a more detailed description of the present invention. The above and other objects, features and advantages of the present invention will be apparent to those skilled in the art from the detailed description of the present invention.
Example 1
Dispersing 17 g of red phosphorus and 0.17 g of sodium dodecyl benzene sulfonate in 500 mL of water, adding 21 g of cyanuric acid and 18.5 g of zinc oxide, and stirring at 85 ℃ for reaction for 3 hours; and adding 15 g of zinc acetate and 40 g of 2-methylimidazole, continuously stirring for reacting for 10 hours, and dehydrating and drying the precipitate obtained by the reaction to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials, wherein the content of red phosphorus is 25%.
Example 2
Dispersing 17 g of red phosphorus and 0.1 g of lauryl sodium sulfate in 600 mL of water, adding 14.5 g of cyanuric acid and 11.5 g of zinc oxide, and reacting for 6 hours at 70 ℃ with stirring; and adding 20.5 g of zinc nitrate and 70 g of 2-methylimidazole, continuously stirring for reacting for 20 hours, and dehydrating and drying the precipitate obtained by the reaction to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials, wherein the content of red phosphorus is 28%.
Example 3
Dispersing 17 g of red phosphorus and 0.3 g of polyvinylpyrrolidone in 500 mL of water, and stirring and reacting 28 g of cyanuric acid and 26 g of zinc oxide at 95 ℃ for 2 h; and adding 9 g of zinc sulfate and 18 g of 2-methylimidazole, continuously stirring for reacting for 6 hours, and dehydrating and drying the precipitate obtained by the reaction to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials, wherein the content of red phosphorus is 23%.
Comparative example 1
Dispersing 17 g of red phosphorus and 0.17 g of sodium dodecyl benzene sulfonate in 500 mL of water, adding 31.5 g of cyanuric acid and 29.5 g of zinc oxide, stirring and reacting at 85 ℃ for 13 h, dehydrating and drying precipitates obtained by the reaction to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate as a single capsule wall material, wherein the content of red phosphorus is 25%.
Comparative example 2
Dispersing 17 g of red phosphorus and 0.17 g of sodium dodecyl benzene sulfonate in 500 mL of water, adding 50.5 g of zinc acetate and 135 g of 2-methylimidazole, stirring at 85 ℃ for reaction for 13 h, dehydrating and drying a precipitate obtained by the reaction to obtain the whiteness red phosphorus flame retardant taking ZIF-8 as a single capsule wall material, wherein the content of red phosphorus is 25%.
Performance test experiments:
the whiteness-improved red phosphorus flame retardant samples prepared in examples 1-3, comparative examples 1 and 2 were subjected to the following tests:
and (3) whiteness testing: weighing 10.00 g of sample, tabletting, placing in a sample box, and testing on a digital display whiteness instrument, wherein the results are shown in table 1;
and (3) oxidation resistance test: respectively weighing 10.00 g of sample in a three-neck flask containing 200 ml of distilled water, boiling the solution for 1 hour, filtering, removing initial filtrate, adding 10.00 g of analytically pure sodium chloride into 100 ml of the filtrate, titrating oxyacid formed by oxidation in the filtrate by using a standard sodium hydroxide solution after dissolution, and expressing the oxidation resistance of oxyacid by the milligrams of sodium hydroxide consumed by each gram of red phosphorus, wherein the results are shown in table 1;
limiting oxygen index test: the test was carried out according to the method of GB/T2406.2-2009, and the addition amount of the coated red phosphorus flame retardant was 12%, and the results are shown in Table 1.
From the test results of examples 1-3 in table 1, it can be seen that the whiteness red phosphorus flame retardant using zinc cyanurate and ZIF-8 as composite capsule wall materials has higher whiteness and flame retardant efficiency, and better oxidation resistance. According to the test results of the example 1, the comparative example 1 and the comparative example 2, the flame retardant performance and the whiteness of the whiteness red phosphorus using the zinc cyanurate and the ZIF-8 as the composite capsule wall materials are obviously better than those of the whiteness red phosphorus sample using the zinc cyanurate or the ZIF-8 as the single capsule wall materials under the condition of the same red phosphorus content. The results show that the zinc cyanurate and the ZIF-8 are used as the composite capsule wall material of the whiteness red phosphorus, the advantages of the zinc cyanurate and the ZIF-8 can be effectively combined, and the zinc cyanurate and the ZIF-8 have good synergistic effect.
It should be understood that although the present invention has been clearly illustrated by the foregoing examples, various changes and modifications may be made therein by those skilled in the art without departing from the spirit and scope of the invention, and it is intended to cover all such changes and modifications as fall within the scope of the appended claims.
Claims (9)
1. A preparation method of a whiteness red phosphorus flame retardant is characterized by comprising the following steps:
(1) dispersing red phosphorus and a dispersing agent in water, adding cyanuric acid and zinc oxide, and reacting for 2-6 h;
(2) adding soluble zinc salt and 2-methylimidazole, reacting for 6-30 h, and dehydrating and drying the precipitate to obtain the whiteness red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials.
2. The preparation method of the whiteness-modified red phosphorus flame retardant according to claim 1, wherein the dispersant is sodium dodecyl benzene sulfonate, sodium dodecyl sulfate or polyvinylpyrrolidone, and the mass ratio of the dispersant to red phosphorus is 0.5-3: 100.
3. the preparation method of the whiteness red phosphorus flame retardant according to claim 1, wherein the reaction temperature is 70-100 ℃.
4. The preparation method of the whiteness-modified red phosphorus flame retardant according to claim 1, wherein the molar ratio of cyanuric acid to red phosphorus is 0.2-0.4: 1.
5. the preparation method of the whiteness red phosphorus flame retardant according to claim 1, wherein the molar ratio of the cyanuric acid to the zinc oxide is 2-2.3: 3.
6. the method for preparing a whitened red phosphorus flame retardant according to claim 1, wherein the zinc salt is zinc acetate, zinc nitrate, zinc chloride, or zinc sulfate.
7. The method for preparing the whiteness red phosphorus flame retardant according to claim 1, wherein Zn is contained in the zinc salt 2+ The molar ratio of the red phosphorus to the red phosphorus is 0.1-0.2: 1.
8. the method for preparing a whitened red phosphorus flame retardant according to claim 1, characterized in that,zn in the zinc salt 2+ The molar ratio to 2-methylimidazole is 1: 3 to 9.
9. A whiteness red phosphorus flame retardant which is prepared by the method of any one of claims 1 to 8, and is characterized in that red phosphorus is compositely coated by zinc cyanurate and ZIF-8.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210796183.7A CN115109316A (en) | 2022-07-07 | 2022-07-07 | Whiteness red phosphorus fire retardant and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210796183.7A CN115109316A (en) | 2022-07-07 | 2022-07-07 | Whiteness red phosphorus fire retardant and preparation method thereof |
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| CN115109316A true CN115109316A (en) | 2022-09-27 |
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| CN202210796183.7A Pending CN115109316A (en) | 2022-07-07 | 2022-07-07 | Whiteness red phosphorus fire retardant and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131175A (en) * | 2011-11-25 | 2013-06-05 | 上海日之升新技术发展有限公司 | Low smoke halogen-free flame retardant reinforced nylon composite material and manufacture method |
| CN107987745A (en) * | 2017-12-08 | 2018-05-04 | 广东莱尔新材料科技股份有限公司 | A kind of halogen-free flame-retardant hot-melt adhesive film on high-frequency transmission wire rod |
| US20200148954A1 (en) * | 2017-07-24 | 2020-05-14 | Adeka Corporation | Composition and flame-retardant resin composition |
| CN112409641A (en) * | 2020-11-06 | 2021-02-26 | 邵阳市富森阻燃材料有限公司 | Zeolite imidazole ester framework material coated red phosphorus flame retardant and preparation method thereof |
-
2022
- 2022-07-07 CN CN202210796183.7A patent/CN115109316A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131175A (en) * | 2011-11-25 | 2013-06-05 | 上海日之升新技术发展有限公司 | Low smoke halogen-free flame retardant reinforced nylon composite material and manufacture method |
| US20200148954A1 (en) * | 2017-07-24 | 2020-05-14 | Adeka Corporation | Composition and flame-retardant resin composition |
| CN107987745A (en) * | 2017-12-08 | 2018-05-04 | 广东莱尔新材料科技股份有限公司 | A kind of halogen-free flame-retardant hot-melt adhesive film on high-frequency transmission wire rod |
| CN112409641A (en) * | 2020-11-06 | 2021-02-26 | 邵阳市富森阻燃材料有限公司 | Zeolite imidazole ester framework material coated red phosphorus flame retardant and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 童涵: "纳微化红磷的有机/无机双层包覆化及其阻燃性能研究", 山东化工, vol. 49, no. 6, pages 61 - 69 * |
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Application publication date: 20220927 |