CN107141509B - A kind of high-performance melamine cyanurate and preparation method thereof - Google Patents

A kind of high-performance melamine cyanurate and preparation method thereof Download PDF

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CN107141509B
CN107141509B CN201710478170.4A CN201710478170A CN107141509B CN 107141509 B CN107141509 B CN 107141509B CN 201710478170 A CN201710478170 A CN 201710478170A CN 107141509 B CN107141509 B CN 107141509B
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melamine cyanurate
parts
performance
melamine
slurry
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CN107141509A (en
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刘大才
杨劲松
杨滨
王洪志
詹强
陈德金
吴雨庭
刘泽祥
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Shifang City Changfeng Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477Six-membered rings
    • C08K5/3492Triazines
    • C08K5/34928Salts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • 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)
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Abstract

The present invention relates to polymer materials flame retardant technical field, a kind of high-performance melamine cyanurate and preparation method thereof is provided.The high-performance melamine cyanurate, raw material include melamine, cyanuric acid, modifying agent and ammonium hydroxide;The advantages that high-performance melamine cyanurate has thermal stability good, and flame retarding efficiency is high, good dispersion.The preparation method of the high-performance melamine cyanurate, comprising: reacted after mixing above-mentioned melamine, cyanuric acid, modifying agent and ammonium hydroxide, obtain slurry;Slurry is subjected to spray drying and cyclonic separation.This method, which can be avoided, damages the crystal of melamine cyanurate, and high production efficiency, it is with short production cycle, preparation process is simple, the product mechanical property and flame retardant property being prepared are splendid, the high-performance melamine cyanurate of addition 6%, flame retardant rating reach UL94V0 grades in nylon 6.

Description

A kind of high-performance melamine cyanurate and preparation method thereof
Technical field
The invention belongs to polymer materials flame retardant technical fields, specifically, being related to a kind of high-performance melamine cyanogen Lithate and preparation method thereof.
Background technique
Melamine cyanurate is widely used in polyamide-based engineering plastics industry as halogen-free flame retardants, is a kind of important Nitrogenated flame retardant.With being continuously increased for the dosages such as engineering plastics, chemical building material, the expansion of high molecular material application field, Flame retardant regulation will be gradually perfect, and the demand of nitrogenated flame retardant will increase rapidly, this is also the exploitation of melamine cyanurate Good opportunity is provided with application.Domestic production capacity in 2013 has had reached 50000t, yield about 30000t, domestic consumption About 20000t.
The product processes have liquid phase method and solid phase method at present, and wherein liquid phase method is prevailing technology.This method exist with Lower disadvantage: reaction rate is slower, and the reaction time is usually at two hours or more;Technique is relative complex, most reaction mother liquor need by Filter, is dry, crushing and etc., the original crystal structure of melamine cyanurate can be destroyed;Product solid content in reaction system Low, solid content is generally in 10-20%;It is high to react viscosity, reaches 10000 centipoises or more, requires height to technique is mixed; Home products flame retardant property is general, and addition 10~12% can just meet that UL94V0 is fire-retardant to be wanted generally in the polyamide 6 (nylon 6) It asks.
Summary of the invention
For deficiency above-mentioned in the prior art, the first object of the present invention is to provide a kind of high-performance melamine cyanogen Lithate.The high-performance melamine cyanurate has thermal stability good, and flame retarding efficiency is high, good dispersion, and comprehensive performance is excellent The advantages that.
The second object of the present invention is to provide a kind of preparation method of high-performance melamine cyanurate, this method energy It enough avoids damaging the crystal of melamine cyanurate, and high production efficiency, with short production cycle, preparation process is simple, The product mechanical property and flame retardant property being prepared are splendid.
In order to achieve the above object, the preferred solution that the present invention uses is:
A kind of high-performance melamine cyanurate, is made of raw material, raw material according to parts by weight, including melamine 100-110 parts, 100-110 parts of cyanuric acid, 3-15 parts of modifying agent and 350-800 parts of ammonium hydroxide.
Further, in preferred embodiments of the present invention, by mass percentage, melamine, cyanuric acid and change Property agent accounts for the 25-33% of raw material summation.
Further, in preferred embodiments of the present invention, according to parts by weight, modifying agent is 6-13.8 parts.
Further, in preferred embodiments of the present invention, modifying agent includes diatomite, white carbon black, one acyl of cyanuric acid Amine, ammeline, melamine polyphosphate, silane coupling agent, fatty alcohol polyoxyethylene ether, aliphatic acid polyethenoxy At least two in ester, polyoxyethylene sorbitan monooleate.
Further, in preferred embodiments of the present invention, by mass percentage, modifying agent includes diatomite 30- 50%, ammelide 1-10%, ammeline 10-45%, silane coupling agent 0.05-5%.
Further, in preferred embodiments of the present invention, ammonia concn 0.5%-10%.
Further, in preferred embodiments of the present invention, ammonia concn 2%-7%.
Further, in preferred embodiments of the present invention, the granularity of high-performance melamine cyanurate is D50= 0.6-1.5 μm, D98=1.8-3.5 μm.
A kind of preparation method of above-mentioned high-performance melamine cyanurate, comprising the following steps: by melamine, trimerization Cyanic acid, modifying agent and ammonium hydroxide are mixed to form mixture in parts by weight;It in temperature is 90-110 DEG C by mixture, pressure is 0.1-1Mpa, mixing speed react 0.5-2.5h under conditions of being 100-400r/min, obtain slurry;Slurry is done by spraying Dry and cyclonic separation.
Further, in preferred embodiments of the present invention, by mass percentage, the content of solid is 20- in slurry 35%.
A kind of beneficial effect of high-performance melamine cyanurate provided by the invention and preparation method thereof is:
(1) high-performance melamine cyanurate provided in an embodiment of the present invention, raw material include melamine, melamine Acid, modifying agent and ammonium hydroxide;In embodiments of the present invention, the melamine, cyanuric acid of use are technical grade, melamine matter Measure degree 99.8%, cyanuric acid mass percentage content 98.5%;
Wherein, melamine is a kind of azacyclo- organic compound produced using urea as raw material, is white single under room temperature Oblique Crystal, without significant peculiar smell.It is currently used primarily in timber processing, plastics, coating, papermaking, adhesive, weaving, leather, electricity In the production processes such as device, medicine, fire retardant.
Cyanuric acid can be used for synthesizing chlorinated derivative, sym-closene;Sodium dichloro cyanurate or potassium;For closing At cyanuric acid-formaldehyde resin;Epoxy resin;Antioxidant;Coating;Adhesive;Pesticide herbicide;Metal cyanide corrosion inhibiter;High score Sub- material modification agent etc..
In embodiments of the present invention, the addition of modifying agent can assist the partial size of control melamine cyanurate, thus It is prepared that a kind of viscosity is lower, more flowability, the preferable slurry of mechanical property;
In embodiments of the present invention, modifying agent preferably includes diatomite, white carbon black, ammelide, cyanuric acid Diamides, melamine polyphosphate, silane coupling agent, fatty alcohol polyoxyethylene ether, polyoxyethylene carboxylate, polyoxyethylene At least two in Sorbitan Monooleate;In the present embodiment, in order to further decrease the viscosity of slurry, slurry is improved Mobility, preferably, by mass percentage, modifying agent includes diatomite 30-50%, ammelide 1- 10%, ammeline 10-45%, silane coupling agent 0.05-5%, the ratio range are tried by inventor's creativeness It tests to obtain, can be synergistic between each modifier raw material in the ratio range, further it is prepared that viscosity is low, flowing The good slurry of property.
Ammonium hydroxide using ammonia spirit as reaction medium, can be improved melamine cyanurate in embodiments of the present invention The yield and purity of salt, obtain that product granularity is uniform, and purity is higher, and solid content is higher.
(2) ratio range of each raw material of high-performance melamine cyanurate provided in an embodiment of the present invention is " raw material According to parts by weight, including 100-110 parts of melamine, 100-110 parts of cyanuric acid, 3-15 parts of modifying agent and ammonium hydroxide 350- 800 parts ", which is to test to obtain by inventor's creativeness, in the ratio range, is able to carry out between each raw material It farthest reacts, reduces the waste of raw material, the production of melamine cyanurate is carried out using the ratio, enables to produce Unreacted melamine is less than 0.1% in product, and unreacted cyanuric acid is less than 0.1%;
Wherein, preferably, modifying agent is 6-13.8 parts, and the further limitation of the amount ranges of modifying agent can be into one Step reduces the viscosity of slurry, improves the mobility of slurry;And it is 25-33% ", solid that solid, which accounts for the mass percent of solid-liquid summation, The mass percent for accounting for solid-liquid summation can assist reducing the viscosity for generating slurry;In embodiments of the present invention, ammonia concn is 0.5%-10%, the ammonium hydroxide in the concentration range can further increase the yield and purity of melamine cyanurate, excellent Selection of land, when ammonia concn is 0.5%-10%, the yield and purity for the melamine cyanurate being prepared are best.
(3) preparation method of high-performance melamine cyanurate provided in an embodiment of the present invention, the preparation method include: Melamine, cyanuric acid, modifying agent and ammonium hydroxide are first mixed to form mixture in parts by weight;It is in temperature by mixture again 90-110 DEG C, pressure 0.1-1MPa, mixing speed react 0.5-2.5h under conditions of being 100-400r/min, obtain slurry, It should be noted that in embodiments of the present invention, by mass percentage, the content of solid is 20-35% in slurry, this is higher Solid content obtain obtained by the selection of easily prepared process conditions and raw material and the proportion collective effect of each raw material;Then Slurry is directly carried out to spray drying and cyclonic separation, high-performance melamine cyanurate product is made, it should be noted that In embodiments of the present invention, the granularity for the high-performance melamine cyanurate being prepared is D50=0.6-1.5 μm, D98 =1.8-3.5 μm, this, which has benefited from production technology used in the embodiment of the present invention, can be avoided conventional size reduction in the process to melamine It is destroyed caused by amine cyanurate crystal, the granularity of obtained melamine cyanurate is excellent;In view of protecting environment, do not make At environmental pollution, it is preferable that in embodiments of the present invention, then washed to tail gas, qualified discharge after pickling;Water lotion supplement The recycling of part ammonia, the concentrated crystallizing and drying of pickling solution obtain ammonium salt.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase Product.
Embodiment 1
A kind of high-performance melamine cyanurate, raw material according to parts by weight, including 100 parts of melamine, trimerization 103 parts of cyanic acid, modifying agent (modifying agent composition: diatomite 44.5%, ammelide 10%, ammeline 45%, 3- aminopropyltriethoxy diethoxy silane 0.5%) 3 parts and 800 parts of ammonium hydroxide.
A kind of preparation method of high-performance melamine cyanurate, comprising the following steps:
100 parts of the above melamine is weighed, 103 parts of cyanuric acid, 3 parts of mixings of modifying agent form material;Separately take 0.5% ammonia 800 parts of water;First ammonium hydroxide is added in low pressure reaction kettle, unlatching stirs at low speed, and the material after mixing is slowly added to from feed opening Reaction kettle;Material accounts for the 20.4% of raw material summation;After adding material, feed opening is closed, is warming up to 90 DEG C, controls pressure 0.1MPa, Mixing speed rises to 100r/min, reacts 0.5h, forms slurry;Slurry is released, its grain graininess and solid content are surveyed, is tested It the results are shown in Table 1;Again by slurry is spray-dried and cyclonic separation, melamine cyanurate product is obtained;Survey gained melamine The ingredient and granularity of cyanurate, test result are shown in Table 1.
Embodiment 2
A kind of high-performance melamine cyanurate, raw material according to parts by weight, including 110 parts of melamine, trimerization 115 parts of cyanic acid, modifying agent (modifying agent composition: diatomite 40%, ammelide 10%, ammeline 45%, 3- aminopropyltriethoxy diethoxy silane 5%) 15 parts and 450 parts of ammonium hydroxide.
A kind of preparation method of high-performance melamine cyanurate, comprising the following steps:
110 parts of the above melamine is weighed, 115 parts of cyanuric acid, 15 parts of mixings of modifying agent form material;Separately take 7% ammonia 450 parts of water;First ammonium hydroxide is added in low pressure reaction kettle, unlatching stirs at low speed, and the material after mixing is slowly added to from feed opening Reaction kettle;Material accounts for the 34.8% of raw material summation;After adding material, feed opening is closed, is warming up to 90 DEG C, controls pressure 0.1MPa, Mixing speed rises to 200r/min, reacts 2h, forms slurry;Slurry is released, its grain graininess and solid content, test knot are surveyed Fruit is shown in Table 1;Again by slurry is spray-dried and cyclonic separation, melamine cyanurate product is obtained;Survey gained melamine cyanogen The ingredient and granularity of lithate, test result are shown in Table 1.
Embodiment 3
A kind of high-performance melamine cyanurate, raw material according to parts by weight, including 105 parts of melamine, trimerization 110 parts of cyanic acid, modifying agent (modifying agent composition: diatomite 44%, ammelide 10%, ammeline 45%, 3- aminopropyltriethoxy diethoxy silane 1%) 13.8 parts and 465 parts of ammonium hydroxide.
A kind of preparation method of high-performance melamine cyanurate, comprising the following steps:
105 parts of the above melamine is weighed, 110 parts of cyanuric acid, 13.8 parts of mixings of modifying agent form material;Separately take 2% 465 parts of ammonium hydroxide;First ammonium hydroxide is added in low pressure reaction kettle, unlatching stirs at low speed, and the material after mixing is slowly added from feed opening Enter reaction kettle;Material accounts for the 33.0% of raw material summation;After adding material, feed opening is closed, is warming up to 90 DEG C, controls pressure 0.1MPa, mixing speed rise to 300r/min, react 2.5h, form slurry;Slurry is released, its grain graininess is surveyed and solid contains Amount, test result are shown in Table 1;Again by slurry is spray-dried and cyclonic separation, melamine cyanurate product is obtained;Survey gained three The ingredient and granularity of poly cyanamid cyanurate, test result are shown in Table 1.
Embodiment 4
A kind of high-performance melamine cyanurate, raw material according to parts by weight, including 115 parts of melamine, trimerization 120 parts of cyanic acid, modifying agent (modifying agent composition: diatomite 44.5%, ammelide 10%, ammeline 45%, 3- aminopropyltriethoxy diethoxy silane 0.5%) 10 parts and 600 parts of ammonium hydroxide.
A kind of preparation method of high-performance melamine cyanurate, comprising the following steps:
115 parts of the above melamine is weighed, 120 parts of cyanuric acid, 10 parts of mixings of modifying agent form material;Separately take 5% ammonia 600 parts of water;First ammonium hydroxide is added in low pressure reaction kettle, unlatching stirs at low speed, and the material after mixing is slowly added to from feed opening Reaction kettle;Material accounts for the 29.0% of raw material summation;After adding material, feed opening is closed, is warming up to 95 DEG C, controls pressure 0.3MPa, Mixing speed rises to 300r/min, reacts 2.0h, forms slurry;Slurry is released, its grain graininess and solid content are surveyed, is tested It the results are shown in Table 1;Again by slurry is spray-dried and cyclonic separation, melamine cyanurate product is obtained;Survey gained melamine The ingredient and granularity of cyanurate, test result are shown in Table 1.
Comparative example 1
Traditional handicraft preparation melamine cyanurate: its raw material according to parts by weight, including 50 parts of melamine, 50 parts of cyanuric acid, 900 parts of water.
The preparation method of the melamine cyanurate of traditional handicraft preparation: 800 parts of water are first added in a kettle, then 100 parts of cyanuric acids are added, stirring is warming up to 90 DEG C or so, 100 parts of melamines are added, is warming up to 100 DEG C, is stirred to react 4h generates the slurry of melamine cyanurate, slurry is released, and surveys its grain graininess and solid content, and test result is shown in Table 1;Slurry is successively filtered, is dried, crushes acquisition melamine cyanurate product.Survey gained melamine cyanurate at Divide and granularity, test result are shown in Table 1.
Comparative example 2
Ammonia-water systems preparation melamine cyanurate: its raw material according to parts by weight, including 100 parts of melamine, 103 parts of cyanuric acid, 800 parts of ammonium hydroxide.
The preparation method of the melamine cyanurate of ammonia-water systems preparation: 800 part of 5% ammonia is first added in a kettle Then water adds 103 parts of cyanuric acids, stirring is warming up to 90 DEG C or so, 100 parts of melamines are added, and is warming up to 95 DEG C, stirring 2h is reacted, the slurry of melamine cyanurate is generated, slurry is released, survey its grain graininess and solid content, test result It is shown in Table 1;Slurry is successively filtered, is dried, crushes acquisition melamine cyanurate product.Survey gained melamine cyanurate Ingredient and granularity, test result be shown in Table 1.
The slurry property and melamine cyanurate property of table 1 embodiment 1-5 and comparative example 1-2 compares
Should the result shows that, the raw material components and preparation process of melamine cyanurate provided by the present invention are prepared The purity of melamine cyanurate, dispersibility and mobility are superior to the trimerization that traditional method and raw material components are prepared Cyanamide cyanurate;
Application experiment
The melamine cyanurate that Example 1-4 and comparative example 1-2 are prepared respectively, with 6 parts of melamine cyanogen Uric acid is added in 94 parts of PA6 after mixing, with pelletizing is squeezed out in double screw extruder, is then added to double-screw injection molding after drying In machine, melting blending is molded into standard sample, carries out performance detection respectively to it, wherein tensile strength (MPa) uses ISO527~2, elongation at break (%) use ISO527~2, and flame retardant rating uses UL94 testing vertical flammability, testing result It is shown in Table 2.
The application performance comparison of the melamine cyanurate of table 2 1-4 of the embodiment of the present invention and comparative example 1-2 preparation
Using the melamine cyanurea being prepared in the ratio range of formula provided in an embodiment of the present invention and each component The advantages such as hydrochlorate has thermal stability good, and flame retarding efficiency is high, good dispersion, and comprehensive performance is excellent;This prepares melamine cyanurate The method of salt, high production efficiency is with short production cycle, and preparation process is simple, the product mechanical property and flame retardant property being prepared It is splendid.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts Every other embodiment, shall fall within the protection scope of the present invention.

Claims (8)

1. a kind of high-performance melamine cyanurate, it is characterized in that: being made of raw material, the raw material according to parts by weight, is wrapped Include 100-110 parts of melamine, 100-110 parts of cyanuric acid, 3-15 parts of modifying agent and 350-800 parts of ammonium hydroxide;By quality percentage Than meter, the modifying agent include diatomite 30-50%, ammelide 1-10%, ammeline 10-45%, Silane coupling agent 0.05-5%.
2. high-performance melamine cyanurate according to claim 1, it is characterized in that: by mass percentage, it is described Melamine, the cyanuric acid and the modifying agent account for the 25-33% of the raw material summation.
3. high-performance melamine cyanurate according to claim 1, it is characterized in that: according to parts by weight, it is described to change Property agent be 6-13.8 parts.
4. high-performance melamine cyanurate according to claim 1, it is characterized in that: the ammonia concn is 0.5%- 10%.
5. high-performance melamine cyanurate according to claim 4, it is characterized in that: the ammonia concn is 2%- 7%.
6. high-performance melamine cyanurate according to claim 1, it is characterized in that: the high-performance melamine cyanogen The granularity of lithate is D50=0.6-1.5 μm, D98=1.8-3.5 μm.
7. a kind of preparation method of high-performance melamine cyanurate as claimed in any one of claims 1 to 6, feature It is: the following steps are included:
Melamine, cyanuric acid, modifying agent and ammonium hydroxide are mixed to form mixture by the parts by weight;By the mixture 0.5-2.5h is reacted under conditions of temperature is 90-110 DEG C, pressure 0.1-1MPa, mixing speed are 100-400r/min, is obtained To slurry;The slurry is subjected to spray drying and cyclonic separation.
8. the preparation method of high-performance melamine cyanurate according to claim 7, it is characterized in that: pressing quality percentage Than meter, the content of solid is 20-35% in the slurry.
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