CN105968415B - A kind of preparation method of high phosphorus content cladded type red phosphorus - Google Patents
A kind of preparation method of high phosphorus content cladded type red phosphorus Download PDFInfo
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- CN105968415B CN105968415B CN201610334953.0A CN201610334953A CN105968415B CN 105968415 B CN105968415 B CN 105968415B CN 201610334953 A CN201610334953 A CN 201610334953A CN 105968415 B CN105968415 B CN 105968415B
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- red phosphorus
- auxiliary agent
- water
- phosphorus
- cladded type
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000011574 phosphorus Substances 0.000 title claims abstract description 24
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910001868 water Inorganic materials 0.000 claims abstract description 34
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 6
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 238000009991 scouring Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 7
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 6
- 239000003063 flame retardant Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- CMQUQOHNANGDOR-UHFFFAOYSA-N 2,3-dibromo-4-(2,4-dibromo-5-hydroxyphenyl)phenol Chemical compound BrC1=C(Br)C(O)=CC=C1C1=CC(O)=C(Br)C=C1Br CMQUQOHNANGDOR-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 238000002036 drum drying Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- MRJCGEZOFMJZCG-UHFFFAOYSA-N C(C1CO1)OC1=CC=C(C=C1)C(C)(C)C1=CC=C(C=C1)OCC1CO1.[Br] Chemical compound C(C1CO1)OC1=CC=C(C=C1)C(C)(C)C1=CC=C(C=C1)OCC1CO1.[Br] MRJCGEZOFMJZCG-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical group O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- 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 discloses a kind of preparation method of high phosphorus content cladded type red phosphorus, red phosphorus and water are positioned in ball mill, are ground；Ground red phosphorus aqueous solution is transferred in Scattered Kettle, puts into auxiliary agent I, adjusts pH, after going water removal phase, water is added and is washed；Auxiliary agent II is added into Scattered Kettle, pH value is adjusted, adds mixed auxiliary agent III, maintains the temperature at 85 ~ 95 DEG C, 2 ~ 3h is reacted, obtains red phosphorus reaction solution；After 7 ~ 9h of red phosphorus reaction solution natural cooling, it is transferred to centrifuge and is centrifuged, product is dried after centrifugation, and high phosphorus content cladded type red phosphorus product is finally made.Its product has the advantages that ignition point is high, red phosphorus content is high, dispersion effect is good.
Description
Technical field
The present invention relates to a kind of preparation method of cladded type red phosphorus, and in particular to a kind of system of high phosphorus content cladded type red phosphorus
Preparation Method.
Background technology
Red phosphorus has been widely used in the polymeric materials such as plastics, rubber as a kind of excellent fire retardant, but red
There are many drawbacks in practical applications for phosphorus.For example, in process of production, as a small amount of yellow phosphorus is remained in the red phosphorus of raw material, make
It is relatively low, inflammable to obtain its burning point；And yellow phosphorus oxidation generation acid easy to moisture absorption and etching apparatus, while produce hypertoxicity gas phosphatization
Hydrogen, so as to shorten service life of equipment, threaten operating personnel's personal safety, pollution environment etc.；In addition, red phosphorus is as inorganic matter,
It is not easy to disperse in organic polymer, therefore, organically-modified processing need to be carried out to red phosphorus surface, while it is difficult to reduce red phosphorus storage
Degree, greatlys save production cost.
Domestic relevant report has：CN101684186A, which is disclosed, first passes through the metal salts such as magnesium, aluminium, zinc and water reaction in red phosphorus
Surface forms metal hydroxides clad, then carries out organic coating by resin bed, but since the cladding number of plies is more, so as to lead
Cause available phosphorus content is relatively low, and fire resistance is had a greatly reduced quality；Existed 201210282927.X disclosing by melamine and formaldehyde
Melamino-formaldehyde glue is formed under alkaline condition to coat red phosphorus, but poor compatibility, difficult scattered and be also easy to produce low occurs
The problems such as molecule formaldehyde.Tetrabromobisphenol A bisglycidyl ether can be applied to plastics, rubber etc. as single fire retardant in itself
In field.
Accordingly, it is desirable to provide a kind of new technical solution solves the above problems.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of high phosphorus content cladded type red phosphorus, by this method
The red phosphorus of preparation has the advantages that ignition point is high, red phosphorus content is high, dispersion effect is good.
In order to solve the above technical problems, a kind of preparation method of high phosphorus content cladded type red phosphorus of present invention offer, including with
Lower step：
（1）Red phosphorus and water are positioned in ball mill, are ground, wherein the mass ratio of red phosphorus and water is 1：2.5~3.5；
（2）Ground red phosphorus aqueous solution is transferred in Scattered Kettle, puts into auxiliary agent I, adjusts pH value to 12 ~ 14, heating
Being stood after to 85 ~ 95 DEG C, 20 ~ 24h of stirring, after going water removal phase, add water and washed, water mutually removes, and is repeated 2 times, wherein
The mass ratio of red phosphorus and water scouring water is 1：1~1.5；
（3）Auxiliary agent II is added into Scattered Kettle, pH value is adjusted to 7 ~ 8, adds mixed auxiliary agent III, keep temperature
Degree is at 85 ~ 95 DEG C, 2 ~ 3h of reaction, and the mass ratio of red phosphorus and auxiliary agent III is 1：0.02 ~ 0.03, obtain red phosphorus reaction solution；
（4）After 7 ~ 9h of red phosphorus reaction solution natural cooling, it is transferred to centrifuge and is centrifuged, product is done after centrifugation
It is dry, high phosphorus content cladded type red phosphorus product is finally made.
Step（2）The auxiliary agent I of middle addition is the sulfurous that the NaOH aqueous solutions that mass concentration is 48% are 30% with mass concentration
The mixed solution of acid sodium aqueous solution, both mass ratioes are 1：0.3~0.4.
Step（3）The auxiliary agent II of middle addition is that mass concentration is 30% biphosphate sodium water solution.
Step（3）The auxiliary agent III of middle addition is the mixed solution of tetrabromobisphenol A bisglycidyl ether and diethylaminopropylamine,
Both mass ratioes are 1:0.3~0.5.
Step（4）Middle centrifuge, is hanging bag type centrifugal machine.
Step（4）Middle drying is using vacuum drum drier.
The present invention uses production technology, the advantage is that：First remaining yellow phosphorus in red phosphorus is removed, then with fire retardant four
Bromine bisphenol-A bisglycidyl ether is coated as main body clad.This method can improve the burning point of product, extend equipment and use
In the service life, save cost of equipment maintenance, ensure that fire resistance, greatly reduce energy consumption, reduce production cost.
Embodiment
In order to deepen the understanding of the present invention, below the invention will be further described, the embodiment be only used for explain this
Invention, does not restrict the protection scope of the present invention.
Embodiment 1
A kind of preparation method of high phosphorus content cladded type red phosphorus, comprises the following steps：
Step（1）, 144.8kg red phosphorus and 362.9kg aqueous solutions are positioned in ball mill, are ground；
Step（2）, ground red phosphorus aqueous solution is transferred in Scattered Kettle, input 15.3kg mass concentrations are 48%
NaOH aqueous solutions and the sodium sulfite aqueous solution that 4.6kg mass concentrations are 30%, adjust pH value 12 ~ 13, are warming up to 85 DEG C, stirring
Stood after 20h, after going water removal phase, add that 145.3kg water is washed, water mutually removes, be repeated 2 times；
Step（3）, 0.9kg mass concentrations are added into Scattered Kettle for 30% biphosphate sodium water solution, adjust pH value to
7 ~ 8,2.3kg tetrabromobisphenol As bisglycidyl ether and 0.69kg diethylaminopropylamines are added, maintains the temperature at 85 DEG C, reacts 2h；
Step（4）, after red phosphorus aqueous solution natural cooling 7h, it is transferred to hanging bag type centrifugal machine and is centrifuged, produced after centrifugation
Product carry out vacuum drum drying（- 0.09Mpa, 120 DEG C）, finally obtained 145.1kg high phosphorus content cladded type red phosphorus products, phosphorus contain
Amount is detected as 97.3%.
Embodiment 2
A kind of preparation method of high phosphorus content cladded type red phosphorus, comprises the following steps：
Step（1）, 421.3kg red phosphorus and 1471.6kg aqueous solutions are positioned in ball mill, are ground；
Step（2）, ground red phosphorus aqueous solution is transferred in Scattered Kettle, input 46.3kg mass concentrations are 48%
NaOH aqueous solutions and the sodium sulfite aqueous solution that 18.3kg mass concentrations are 30%, adjust pH value 13 ~ 14, are warming up to 95 DEG C, stirring
Stood after 24h, after going water removal phase, add that 630.9kg water is washed, water mutually removes, be repeated 2 times；
Step（3）, 3.9kg mass concentrations are added into Scattered Kettle for 30% biphosphate sodium water solution, adjust pH value to
7 ~ 8,8.4kg tetrabromobisphenol As bisglycidyl ether and 4.2kg diethylaminopropylamines are added, maintains the temperature at 95 DEG C, reacts 3h；
Step（4）, after red phosphorus aqueous solution natural cooling 9h, it is transferred to hanging bag type centrifugal machine and is centrifuged, produced after centrifugation
Product carry out vacuum drum drying（- 0.09Mpa, 120 DEG C）, finally obtained 425.2kg high phosphorus content cladded type red phosphorus products, phosphorus contain
Amount is detected as 96.8%.
Embodiment 3
A kind of preparation method of high phosphorus content cladded type red phosphorus, comprises the following steps：
Step（1）, 314.2kg red phosphorus and 940.7kg aqueous solutions are positioned in ball mill, are ground；
Step（2）, ground red phosphorus aqueous solution is transferred in Scattered Kettle, input 32.8kg mass concentrations are 48%
NaOH aqueous solutions and the sodium sulfite aqueous solution that 12.7kg mass concentrations are 30%, adjust pH value 12 ~ 13, are warming up to 90 DEG C, stirring
Stood after 22h, after going water removal phase, add that 439.7kg water is washed, water mutually removes, be repeated 2 times；
Step（3）, 2.4kg mass concentrations are added into Scattered Kettle for 30% biphosphate sodium water solution, adjust pH value to
7 ~ 8,6.3kg tetrabromobisphenol As bisglycidyl ether and 2.5kg diethylaminopropylamines are added, maintains the temperature at 90 DEG C, reacts 3h；
Step（4）, after red phosphorus aqueous solution natural cooling 9h, it is transferred to hanging bag type centrifugal machine and is centrifuged, produced after centrifugation
Product carry out vacuum drum drying（- 0.09Mpa, 120 DEG C）, finally obtained 320.4kg high phosphorus content cladded type red phosphorus products, phosphorus contain
Amount is detected as 96.1%.
In the present invention, first by red phosphorus and water mixed grinding so that red phosphorus is sufficiently humidified so as to, and is milled uniformly, and prevent from milling
During because temperature rises cause the spontaneous combustion of yellow phosphorus；Auxiliary agent I is added, rear washing carries out removing impurity, and auxiliary agent I is added to
Effective to remove yellow phosphorus, because yellow phosphorus content is different in red phosphorus, the addition of auxiliary agent I is different；It is NaOH water why to select auxiliary agent I
The mixed solution of solution and sodium sulfite aqueous solution, because NaOH aqueous solution costs are relatively low, sodium sulfite aqueous solution is as reduction
Agent, prevents from aoxidizing, removing chlorion in red phosphorus, while red phosphorus is bleached.When adding auxiliary agent I, adjusting pH value to 12 ~
14；
Since alkaline condition can influence the use of follow-up auxiliary agent III, it is water-soluble in order to adjust red phosphorus to add auxiliary agent II later
The pH value of liquid is to 7 ~ 8, and because red phosphorus solution ph is different after washing, the addition of auxiliary agent II is also different.Why auxiliary agent II is selected
For biphosphate sodium water solution, because its pH value is 7 ~ 8, it can prevent red phosphorus aqueous solution from becoming acid, while effectively remove removing chloride；
Add auxiliary agent III to be coated, it is tetrabromobisphenol A bisglycidyl ether and divinyl why to select auxiliary agent III
Triamine, because inherently a kind of fire retardant of tetrabromobisphenol A bisglycidyl ether, can reach synergistic effect and improve with red phosphorus
Fire resistance；Diethylenetriamine may be such that the epoxy group of tetrabromobisphenol A bisglycidyl ether occurs as most common curing agent
Cross-linking reaction, so as to complete the cladding of red phosphorus particle.
Clad outside red phosphorus only has tetrabromobisphenol A bisglycidyl ether to coat one layer with diethylaminopropylamine, clad
Few, available phosphorus content is higher, good flame resistance.
The present invention crosslinks reaction by the epoxy group of tetrabromobisphenol A bisglycidyl ether, completes to red phosphorus particle
Coat, product has the advantages that burning point is high, compatibility is good, fire resistance is good after cladding.
Claims (3)
1. a kind of preparation method of high phosphorus content cladded type red phosphorus, it is characterised in that comprise the following steps：
（1）Red phosphorus and water are positioned in ball mill, are ground, wherein the mass ratio of red phosphorus and water is 1：2.5~3.5；
（2）Ground red phosphorus aqueous solution is transferred in Scattered Kettle, puts into auxiliary agent I, adjust pH value to 12 ~ 14, be warming up to 85 ~
95 DEG C, stirring 20 ~ 24h after stand, go water removal phase after, add water and washed, water mutually removes, and is repeated 2 times, wherein red phosphorus with
The mass ratio of water scouring water is 1：1~1.5；
（3）Auxiliary agent II is added into Scattered Kettle, pH value is adjusted to 7 ~ 8, adds mixed auxiliary agent III, maintain the temperature at
85 ~ 95 DEG C, 2 ~ 3h is reacted, the mass ratio of red phosphorus and auxiliary agent III is 1：0.02 ~ 0.03, obtain red phosphorus reaction solution；
（4）After 7 ~ 9h of red phosphorus reaction solution natural cooling, it is transferred to centrifuge and is centrifuged, product is dried after centrifugation, most
High phosphorus content cladded type red phosphorus product is made eventually；
Step（2）The auxiliary agent I of middle addition is the sodium sulfite that the NaOH aqueous solutions that mass concentration is 48% are 30% with mass concentration
The mixed solution of aqueous solution, both mass ratioes are 1：0.3~0.4；
Step（3）The auxiliary agent II of middle addition is that mass concentration is 30% biphosphate sodium water solution；
Step（3）The auxiliary agent III of middle addition is the mixed solution of tetrabromobisphenol A bisglycidyl ether and diethylaminopropylamine, both
Mass ratio be 1:0.3~0.5.
A kind of 2. preparation method of high phosphorus content cladded type red phosphorus according to claim 1, it is characterised in that：Step（4）
Middle centrifuge, is hanging bag type centrifugal machine.
A kind of 3. preparation method of high phosphorus content cladded type red phosphorus according to claim 1, it is characterised in that：Step（4）
Middle drying is using vacuum drum drier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610334953.0A CN105968415B (en) | 2016-05-19 | 2016-05-19 | A kind of preparation method of high phosphorus content cladded type red phosphorus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610334953.0A CN105968415B (en) | 2016-05-19 | 2016-05-19 | A kind of preparation method of high phosphorus content cladded type red phosphorus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105968415A CN105968415A (en) | 2016-09-28 |
| CN105968415B true CN105968415B (en) | 2018-05-11 |
Family
ID=56957153
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| CN201610334953.0A Expired - Fee Related CN105968415B (en) | 2016-05-19 | 2016-05-19 | A kind of preparation method of high phosphorus content cladded type red phosphorus |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56136846A (en) * | 1980-03-31 | 1981-10-26 | Hitachi Chem Co Ltd | Heat-resistant and flame-retardant resin composition for laminate |
| CN101343542A (en) * | 2008-08-25 | 2009-01-14 | 温州大学 | Method for preparing ultra-fine red phosphorus microcapsule |
| CN102010618A (en) * | 2010-11-19 | 2011-04-13 | 桐城市信得新材料有限公司 | Method for preparing encapsulated red phosphorus |
| CN102140262A (en) * | 2011-01-19 | 2011-08-03 | 成都理工大学 | Preparation method of light-color microcapsule red phosphorus |
-
2016
- 2016-05-19 CN CN201610334953.0A patent/CN105968415B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56136846A (en) * | 1980-03-31 | 1981-10-26 | Hitachi Chem Co Ltd | Heat-resistant and flame-retardant resin composition for laminate |
| CN101343542A (en) * | 2008-08-25 | 2009-01-14 | 温州大学 | Method for preparing ultra-fine red phosphorus microcapsule |
| CN102010618A (en) * | 2010-11-19 | 2011-04-13 | 桐城市信得新材料有限公司 | Method for preparing encapsulated red phosphorus |
| CN102140262A (en) * | 2011-01-19 | 2011-08-03 | 成都理工大学 | Preparation method of light-color microcapsule red phosphorus |
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| Publication number | Publication date |
|---|---|
| CN105968415A (en) | 2016-09-28 |
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