CN104513500A - Preparation method of expansion-type red phosphorus microcapsule - Google Patents
Preparation method of expansion-type red phosphorus microcapsule Download PDFInfo
- Publication number
- CN104513500A CN104513500A CN201310444580.9A CN201310444580A CN104513500A CN 104513500 A CN104513500 A CN 104513500A CN 201310444580 A CN201310444580 A CN 201310444580A CN 104513500 A CN104513500 A CN 104513500A
- Authority
- CN
- China
- Prior art keywords
- red phosphorus
- reactor
- preparation
- microcapsule
- nozzle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a preparation method of an expansion-type red phosphorus microcapsule. The preparation method comprises the following steps: step one, adding red phosphorus, disodium m-phthalate, and m-phenylenediamine dihydrochloride into a high-pressure reactor, and then sealing the reactor; step two, introducing CO2 into the reactor to eliminate the air in the reactor, then adjusting the inlet/outlet valves to make the CO2 go through the reactor in a small flow, and discharging CO2 from the outlet; step three, heating to a required temperature, starting a stirrer, opening a high pressure pump to supply CO2 to maintain the pressure in the reactor, heating to a required temperature, and then carrying out reactions under a constant temperature for a while; step four, after the reaction, closing the gas inlet vale and the gas outlet valve, opening a nozzle, and rapidly ejecting the reaction products into a collecting apparatus through the nozzle so as to obtain the red phosphorus microcapsules. In the provided preparation method, the red phosphorus microcapsule is prepared through a supercritical reaction cladding method, the capsule wall of the prepared red phosphorus microcapsule is more stable and cannot be peeled off easily, and thus the red phosphorus microcapsule has a good application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic phosphorus flame retardant, be specifically related to a kind of preparation method of red phosphorus microcapsule.
Background technology
Advantages such as inorganic phosphorus flame retardant has that fire retarding effect is lasting, Heat stability is good, non-volatile, Halogen and be subject to the favor of user.Red phosphorus such as, because only containing ignition-proof element phosphorus, so higher than the flame retarding efficiency of other phosphorus flame retardants, but there is a lot of shortcoming in red phosphorus: volatility in atmosphere, poor with resin compatible, and long-term contact with air discharges hypertoxic gas PH
3, contaminate environment, easily ignited by impacting, the red-purple of red phosphorus easily makes by its fire-retardant color articles etc.For overcoming above-mentioned shortcoming, red phosphorus microcapsule metallization processes is arisen at the historic moment.
Microencapsulated powder oil ties up to that red phosphorus Surface coating one deck or which floor protective membrane formed, and is a kind of new technology in order to stable red phosphorus.At present, red phosphorus is coated is divided into inorganic coating method, organic coating method and inorganic-organic hybrid cladding process.Organic coating method at present adopt thermosetting resin as resol, melamine resin, furfuryl alcohol resin, aniline resin, epoxy resin and Synolac etc. with interfacial polymerization or in-situ polymerization coated.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of expanded polystyrene veneer red phosphorus microcapsule, make the effect microcapsule wall that obtains more stable, difficult drop-off, has better application prospect advantage.
A preparation method for expanded polystyrene veneer red phosphorus microcapsule, it comprises the following steps:
One, red phosphorus, m-phthalic acid disodium salt and metaphenylene diamine hydrochloride add in autoclave by 1:1:1 in molar ratio, sealing;
Two, CO is passed into
215min, to get rid of the air in reactor, then regulates the size of terminal valve, makes CO
2with less flow by reactor, and discharge in exit;
Three, be warming up to 40 DEG C, start agitator, rotate with the rotating speed of 350-450r/min, and open high-pressure pump and supplement CO
2, the pressure in maintenance reactor, at 18-25MPa, is warming up to 200 DEG C-280 DEG C, isothermal reaction 150-220min;
Four, reacted, closed intake valve and air outlet valve, open nozzle, product is spurted in collection device fast by nozzle, obtains red phosphorus microcapsule.
Expanded polystyrene veneer red phosphorus microcapsule preparation method provided by the invention, its beneficial effect is, adopts red phosphorus microcapsule prepared by supercritical reaction cladding process, cyst wall is more stable, difficult drop-off, has better application prospect advantage.
Embodiment
Below in conjunction with an embodiment, expanded polystyrene veneer red phosphorus microcapsule preparation method provided by the invention is described in detail.
Embodiment
One, 100mol red phosphorus, 100mol m-phthalic acid disodium salt and 100mol metaphenylene diamine hydrochloride are added in autoclave, sealing;
Two, CO is passed into
215min, to get rid of the air in reactor, then regulates the size of terminal valve, makes CO
2with less flow by reactor, and discharge in exit;
When three, being warming up to more than 40 DEG C, starting agitator and rotate with the rotating speed of 400r/min, and open high-pressure pump and supplement a certain amount of CO
2, along with the rising of temperature, the pressure in reactor constantly rises, and when temperature reaches 230 DEG C, controls pressure in reactor at 22MPa, isothermal reaction 180min;
Four, reacted, closed intake valve and air outlet valve, open nozzle, product is spurted in collection device fast by nozzle, obtains red phosphorus microcapsule.
Claims (1)
1. a preparation method for expanded polystyrene veneer red phosphorus microcapsule, is characterized in that: it comprises the following steps:
One, red phosphorus, m-phthalic acid disodium salt and metaphenylene diamine hydrochloride add in autoclave by 1:1:1 in molar ratio, sealing;
Two, CO is passed into
215min, to get rid of the air in reactor, then regulates the size of terminal valve, makes CO
2with less flow by reactor, and discharge in exit;
Three, be warming up to 40 DEG C, start agitator, rotate with the rotating speed of 350-450r/min, and open high-pressure pump and supplement CO
2, the pressure in maintenance reactor, at 18-25MPa, is warming up to 200 DEG C-280 DEG C, isothermal reaction 150-220min;
Four, reacted, closed intake valve and air outlet valve, open nozzle, product is spurted in collection device fast by nozzle, obtains red phosphorus microcapsule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310444580.9A CN104513500A (en) | 2013-09-27 | 2013-09-27 | Preparation method of expansion-type red phosphorus microcapsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310444580.9A CN104513500A (en) | 2013-09-27 | 2013-09-27 | Preparation method of expansion-type red phosphorus microcapsule |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104513500A true CN104513500A (en) | 2015-04-15 |
Family
ID=52789384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310444580.9A Pending CN104513500A (en) | 2013-09-27 | 2013-09-27 | Preparation method of expansion-type red phosphorus microcapsule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104513500A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106065126A (en) * | 2016-08-19 | 2016-11-02 | 广州市丰驰新材料有限公司 | A kind of high concentration high melanism microcapsule coated red phosphorus combustion inhibitor master batch and preparation method thereof |
-
2013
- 2013-09-27 CN CN201310444580.9A patent/CN104513500A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106065126A (en) * | 2016-08-19 | 2016-11-02 | 广州市丰驰新材料有限公司 | A kind of high concentration high melanism microcapsule coated red phosphorus combustion inhibitor master batch and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2012165911A3 (en) | Method for preparing porous organic-inorganic hybrid materials | |
| CN104130685A (en) | Reaction type halogen-free flame-retardant spray polyurea elastomer coating and preparation method thereof | |
| WO2012089940A3 (en) | Device for converting heat energy into mechanical energy | |
| CN205056007U (en) | Toluene diisocyanate seals reaction unit | |
| CN203886765U (en) | Heat-preservation glue tank system for coating bottom layer | |
| CN104513500A (en) | Preparation method of expansion-type red phosphorus microcapsule | |
| CN201892224U (en) | Atomized gasified air-mixed light-hydrocarbon gas preparation device | |
| NZ599816A (en) | An apparatus for generating heat | |
| CN105712865B (en) | Solid citric acid aluminum crosslinker, preparation method and its application | |
| CN202297113U (en) | Chlorine dioxide generator | |
| CN204220354U (en) | A kind of air arm's helmet spray equipment | |
| CN101733053B (en) | Preparation method of immobilized ionic liquid by jet type suspension and dispersion method | |
| CN201676801U (en) | High evenness oil spraying device | |
| CN205137431U (en) | High -efficient oil heating furnace | |
| CN104086448A (en) | Synthesis method of o-amino pheylmethyl ether | |
| CN106146863A (en) | A kind of process preparing Tissuemat E powder | |
| CN102297337A (en) | Application process of steam-to-steam jet flow direct mixing device in conveying of industrial steam of electric power plant | |
| CN207596484U (en) | Two-step method produces the device of aluminium polychloride | |
| CN206348254U (en) | A kind of salt spray tester | |
| CN204097360U (en) | A kind of film fueling injection equipment for composite fertilizer | |
| RU2582446C2 (en) | Method for producing fire extinguishing jet and apparatus for producing fire-extinguishing jet | |
| JP2013183731A (en) | Device for producing carbonated water and spraying fine mist thereof | |
| CN202070461U (en) | Coating thermostatic device | |
| CN204607896U (en) | A kind of guanidoacetic acid production system | |
| CN102975991A (en) | Novel storage tank |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150415 |
|
| WD01 | Invention patent application deemed withdrawn after publication |