CN103382265A - Preparation method of melamine cyanurate fire retardant - Google Patents
Preparation method of melamine cyanurate fire retardant Download PDFInfo
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- CN103382265A CN103382265A CN2013102761182A CN201310276118A CN103382265A CN 103382265 A CN103382265 A CN 103382265A CN 2013102761182 A CN2013102761182 A CN 2013102761182A CN 201310276118 A CN201310276118 A CN 201310276118A CN 103382265 A CN103382265 A CN 103382265A
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Abstract
The invention discloses a preparation method of a melamine cyanurate fire retardant, and belongs to the field of flame-retardant polymeric material preparation. the target product is prepared by taking melamine and cyanuric acid as raw materials, and water as a solvent. The preparation method comprises following steps, more specifically: preparing the raw materials; mixing melamine and cyanuric acid; adding water into a kneader and heating; adding the raw materials into the kneader, and performing reaction; drying; crushing; and weighing and packaging. Technological process and production cycle of the product are short; technologies are simple; water consumption and energy consumption are less; and efficiency is high.
Description
Technical field
The present invention relates to a kind of preparation method of melamine cyanurate flame retardant, belong to the preparation field of flame-proofed polymer material.
Background technology
Fire retardant is the functional aid of giving the combustible polymers flame retardancy, is divided into additive flame retardant and reactive flame retardant according to application mode.According to composition, additive flame retardant mainly comprises inorganic combustion inhibitor, halogenated flame retardant (organic chloride and organic bromide), phosphorus flame retardant (red phosphorus, phosphoric acid ester and halogenated phosphate etc.) and nitrogenated flame retardant etc.The trimeric cyanamide flame retardant is the splendid nitrogenated flame retardant of a kind of application performance, also the good lubricants of plastics simultaneously, compare with phosphorous, halogen-containing flame retardant, trimeric cyanamide cyanogen flame retardant has the advantages such as toxicity is low, flame retarding efficiency is high, suitability is strong, low price, the nontoxic environment-friendly product of melamine series, heat resistance is high, Heat stability is good.After melamine cyanurate adds synthetic resins, can not faded, the product of non-blooming, electrical property and mechanical property excellence; Melamine cyanurate is specially adapted to the fire-retardant of not filled polyamide 6 and 66, flame retardant properties can reach the UL94V-0 level, can be widely used in the fire-retardant of epoxy resin, polyurethane, polypropylene, polymeric amide and rubber item, be particularly suitable for nylon 6 and nylon 66 these two kinds pure nylon uses, can make them easily reach the flame retardant effect of UL94V-0 level, be added in lubricating oil, fat, cream and make solid lubrication additive, be added on and make fire-retardant, delustring auxiliary agent in frie retardant coating, be added on and make lubricant in makeup.It has extremely low application cost, superior various advantages such as electrical property, mechanical property and tinctorial property.
At present, the preparation method of melamine cyanurate has three kinds:
1, Wyler's process: namely when urea pyrolysis becomes cyanuric acid, add trimeric cyanamide to react, or urea and trimeric cyanamide are together carried out heat of solution, single step reaction generates the melamine cyanurate crude product, then boils through acid, the refining melamine cyanurate product that obtains of the operations such as washing, drying, the method raw material is cheap and easy to get, and production cost is low, but severe operational environment, the labour protection measure requires high, has increased subsequent disposal work.
2, high-temperature melting method: the method is that directly directly frit reaction is to generate the method for the high melamine cyanurate of productive rate more than (300 ℃) under hot conditions with reaction raw materials trimeric cyanamide and cyanuric acid, and this method power consumption is large, and reaction time is long.
3, cyanuric acid method: the method is equimolar trimeric cyanamide and cyanuric acid to be placed in water form suspension, stoichiometric number hour, obviously become sticky thick rear continuation reaction for some time until slip at a certain temperature, more after filtration, dry, fragmentation obtains finished product, and mother liquor is recyclable to be recycled.The method technique is simple, and product purity is high, and speed of response is very fast, could be near reaction end but be reacted to certain hour.
At present, the cyanuric acid method is a kind of method of generally using, but the method still exists the reaction times longer, big energy-consuming, and water consumption is large, and the heavier defective of employee's workload.
Summary of the invention
The object of the invention is to provides a kind of preparation method of melamine cyanurate flame retardant for deficiency of the prior art, and the method technique is simple, and life cycle of the product is short, and water consumption is few, consumes energy little.
For solving the problems of the technologies described above, the present invention adopts following technical scheme to realize:
A kind of preparation method of melamine cyanurate flame retardant comprises the steps:
1) raw material mixes: add the cyanuric acid of 14～16 weight parts and 14～16 weight part trimeric cyanamides to mix in mixing machine, mixing time is 25～35 minutes;
2) adding water heats up: add the water of 7～8 weight parts in kneader, be warming up to 65～75 ℃;
3) reaction that feeds intake: mixture is dropped into kneader react, the reaction times is 5～6 hours;
4) oven dry: open the kneading cover, allow the moisture spontaneous evaporation, during oven dry, vapor pressure requires at 3～4 kilograms, and bake out temperature is 100～110 ℃, and drying time is 2 hours;
5) pulverize: with below material crushing to 25 micron;
6) packing of weighing.
In described raw material, the quality percentage composition 99.5% of trimeric cyanamide, the quality percentage composition 99.5% of cyanuric acid.
Beneficial effect of the present invention: technique is simple, and is with short production cycle, and water consumption is few, consumes energy little.
Embodiment
Below in conjunction with specific embodiment, the present invention is elaborated.
, as raw material cyanuric acid 300kg, trimeric cyanamide 300kg are dropped in mixing machine with trimeric cyanamide and cyanuric acid, mix discharging after 30 minutes, with the material special-purpose Shipping Sack of packing into; Then add entry 150kg in kneader, be warming up to 70 ℃, the steam off valve is opened the kneading cover, and mixture is dropped into kneader fast, feed intake complete after, cover kneader, begin the reaction,
Reaction times is 6 hours; After reaction finishes, open the kneading cover, allow the moisture spontaneous evaporation, during oven dry, vapor pressure requires per hour to record pressure one time between 3～4 kilograms, and drying time is 2 hours, oven dry finish kneader wall, stirring rake and under the caking that covers shovels.
Sampling send the laboratory to detect, the packing of weighing, and finished product is pressed gross weight 15.2kg packing.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill of the present invention is modified or is equal to replacement technical scheme of the present invention; and not breaking away from aim and the scope of technical scheme, it all should be encompassed in claim scope of the present invention.
Claims (2)
1. the preparation method of a melamine cyanurate flame retardant, is characterized in that: comprise the steps:
1) raw material mixes: add the cyanuric acid of 14～16 weight parts and 14～16 weight part trimeric cyanamides to mix in mixing machine, mixing time is 25～35 minutes;
2) adding water heats up: add the water of 7～8 weight parts in kneader, be warming up to 65～75 ℃;
3) reaction that feeds intake: mixture is dropped into kneader react, the reaction times is 6 hours;
4) oven dry: open the kneading cover, allow the moisture spontaneous evaporation, during oven dry, vapor pressure is 3～4 kilograms, and bake out temperature is 100～110 ℃, and drying time is 2 hours;
5) pulverize: with below material crushing to 25 micron;
6) packing of weighing.
2. the preparation method of a kind of melamine cyanurate flame retardant according to claim 1 is characterized in that: in described raw material, and the quality percentage composition 99.5% of trimeric cyanamide, the quality percentage composition 99.5% of cyanuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310276118.2A CN103382265B (en) | 2013-07-03 | 2013-07-03 | Preparation method of melamine cyanurate fire retardant |
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| CN201310276118.2A CN103382265B (en) | 2013-07-03 | 2013-07-03 | Preparation method of melamine cyanurate fire retardant |
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| CN103382265A true CN103382265A (en) | 2013-11-06 |
| CN103382265B CN103382265B (en) | 2015-04-01 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496151A (en) * | 2016-10-12 | 2017-03-15 | 古道尔工程塑胶（深圳）有限公司 | A kind of BACN and preparation method thereof |
| CN106588797A (en) * | 2016-11-22 | 2017-04-26 | 广东聚航新材料研究院有限公司 | Method for preparing melamine cyanuric urate flame retardant with ball-milling method |
| CN106700130A (en) * | 2016-12-29 | 2017-05-24 | 湖州利鹏新材料科技有限公司 | Composite modified melamine cyanurate fire retardant and preparation method and application of fire retardant |
| CN108689955A (en) * | 2018-07-24 | 2018-10-23 | 济南泰星精细化工有限公司 | A kind of preparation method of graininess melamine cyanurate |
| CN114751869A (en) * | 2022-04-21 | 2022-07-15 | 山东泰星新材料股份有限公司 | Preparation method of high-dispersion melamine cyanurate flame retardant |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200453A (en) * | 2007-11-30 | 2008-06-18 | 浙江三鼎科技有限公司 | Rapid preparation method of melamine cyanurate flame retardant |
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2013
- 2013-07-03 CN CN201310276118.2A patent/CN103382265B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200453A (en) * | 2007-11-30 | 2008-06-18 | 浙江三鼎科技有限公司 | Rapid preparation method of melamine cyanurate flame retardant |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496151A (en) * | 2016-10-12 | 2017-03-15 | 古道尔工程塑胶（深圳）有限公司 | A kind of BACN and preparation method thereof |
| CN106496151B (en) * | 2016-10-12 | 2019-05-07 | 古道尔工程塑胶（深圳）有限公司 | A kind of fire retardant and preparation method thereof |
| CN106588797A (en) * | 2016-11-22 | 2017-04-26 | 广东聚航新材料研究院有限公司 | Method for preparing melamine cyanuric urate flame retardant with ball-milling method |
| CN106700130A (en) * | 2016-12-29 | 2017-05-24 | 湖州利鹏新材料科技有限公司 | Composite modified melamine cyanurate fire retardant and preparation method and application of fire retardant |
| CN106700130B (en) * | 2016-12-29 | 2019-06-21 | 湖州利鹏新材料科技有限公司 | A kind of composite modified melamine cyanurate flame retardant and its preparation method and application |
| CN108689955A (en) * | 2018-07-24 | 2018-10-23 | 济南泰星精细化工有限公司 | A kind of preparation method of graininess melamine cyanurate |
| CN114751869A (en) * | 2022-04-21 | 2022-07-15 | 山东泰星新材料股份有限公司 | Preparation method of high-dispersion melamine cyanurate flame retardant |
| CN114751869B (en) * | 2022-04-21 | 2024-02-13 | 山东泰星新材料股份有限公司 | Preparation method of high-dispersion melamine cyanurate flame retardant |
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| CN103382265B (en) | 2015-04-01 |
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