CN107141509A - 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 PDFInfo
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- CN107141509A CN107141509A CN201710478170.4A CN201710478170A CN107141509A CN 107141509 A CN107141509 A CN 107141509A CN 201710478170 A CN201710478170 A CN 201710478170A CN 107141509 A CN107141509 A CN 107141509A
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- Prior art keywords
- melamine cyanurate
- performance
- parts
- melamine
- modifying agent
- Prior art date
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- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 239000002002 slurry Substances 0.000 claims abstract description 37
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 34
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 28
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- YSKUZVBSHIWEFK-UHFFFAOYSA-N ammelide Chemical compound NC1=NC(O)=NC(O)=N1 YSKUZVBSHIWEFK-UHFFFAOYSA-N 0.000 claims description 9
- MASBWURJQFFLOO-UHFFFAOYSA-N ammeline Chemical compound NC1=NC(N)=NC(O)=N1 MASBWURJQFFLOO-UHFFFAOYSA-N 0.000 claims description 9
- -1 polyoxyethylene Polymers 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 claims description 4
- MEFUMNTZTUDUBG-UHFFFAOYSA-N oxalonitrile 1,3,5-triazine-2,4,6-triamine Chemical compound N#CC#N.N1=C(N)N=C(N)N=C1N MEFUMNTZTUDUBG-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 229920000388 Polyphosphate Polymers 0.000 claims description 3
- 239000001205 polyphosphate Substances 0.000 claims description 3
- 235000011176 polyphosphates Nutrition 0.000 claims description 3
- 102220043159 rs587780996 Human genes 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 102220112166 rs61747639 Human genes 0.000 claims description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims 1
- 125000005233 alkylalcohol group Chemical group 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000003063 flame retardant Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 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 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 5
- 229920002292 Nylon 6 Polymers 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 3
- 230000000979 retarding effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 13
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical compound OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 238000010792 warming Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000005829 trimerization reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000007973 cyanuric acids Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 150000007974 melamines Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 1
- LBIUOESTBBGQJG-UHFFFAOYSA-N 7,9-dihydro-3H-purine-2,6,8-trione oxalonitrile 1,3,5-triazine-2,4,6-triamine Chemical compound N1=C(N)N=C(N)N=C1N.N1C(=O)NC=2NC(=O)NC2C1=O.N#CC#N LBIUOESTBBGQJG-UHFFFAOYSA-N 0.000 description 1
- SZWMYRXPLPUQQB-UHFFFAOYSA-N C(#N)NC(=O)N.N1=C(N)N=C(N)N=C1N Chemical compound C(#N)NC(=O)N.N1=C(N)N=C(N)N=C1N SZWMYRXPLPUQQB-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- MSFGZHUJTJBYFA-UHFFFAOYSA-M sodium dichloroisocyanurate Chemical compound [Na+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O MSFGZHUJTJBYFA-UHFFFAOYSA-M 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229950009390 symclosene Drugs 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009941 weaving Methods 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
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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)
- Lubricants (AREA)
Abstract
The present invention relates to polymer materials flame retardant technical field, there is provided a kind of high-performance melamine cyanurate and preparation method thereof.The high-performance melamine cyanurate, its raw material includes melamine, cyanuric acid, modifying agent and ammoniacal liquor；The high-performance melamine cyanurate has heat endurance good, and flame retarding efficiency is high, the advantages of good dispersion.The preparation method of the high-performance melamine cyanurate, including：Reacted after above-mentioned melamine, cyanuric acid, modifying agent and ammoniacal liquor are mixed, obtain slurry；Slurry is spray-dried and cyclonic separation.This method can avoid damaging the crystal of melamine cyanurate, and production efficiency is high, it is with short production cycle, preparation process is simple, the product mechanical property and fire resistance prepared is splendid, high-performance melamine cyanurate of addition 6% in nylon 6, flame retardant rating reaches UL94V0 grades.
Description
Technical field
The invention belongs to polymer materials flame retardant technical field, specifically, it is related to a kind of high-performance melamine cyanogen
Lithate and preparation method thereof.
Background technology
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 consumptions such as engineering plastics, chemical building material, the expansion of high polymer material application field,
Flame retardant regulation will be gradually perfect, and the demand of nitrogenated flame retardant will be increased rapidly, and this is also the exploitation of melamine cyanurate
Good opportunity is provided with application.Domestic production capacity in 2013 has reached 50000t, yield about 30000t, domestic consumption
About 20000t.
The current product processes have liquid phase method and solid phase method, and wherein liquid phase method is prevailing technology.This method exist with
Lower shortcoming：Reaction rate is slower, and the reaction time is generally more than two hours；Technique is relative complex, most reaction mother liquor need by
The step such as filter, dry, crushing, can destroy the original crystal structure of melamine cyanurate；Product solids content in reaction system
Low, solids content is typically in 10-20%；React viscosity high, reach more than 10000 centipoises, it is high to mixing technological requirement；
Home products fire resistance is general, typically in polyamide 6 (nylon 6) addition 10~12% can just meet that UL94V0 is fire-retardant will
Ask.
The content 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 heat endurance good, and flame retarding efficiency is high, and good dispersion, combination property is excellent
The advantages of.
The second object of the present invention is to provide a kind of preparation method of high-performance melamine cyanurate, this method energy
Enough avoid damaging the crystal of melamine cyanurate, and production efficiency is high, with short production cycle, preparation process is simple,
The product mechanical property and fire resistance prepared is splendid.
In order to achieve the above object, the preferred solution that uses of the present invention is：
A kind of high-performance melamine cyanurate, is made up of raw material, raw materials by weight portion meter, including melamine
350-800 parts of 100-110 parts, 100-110 parts of cyanuric acid, 3-15 parts of modifying agent and ammoniacal liquor.
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, count by weight, modifying agent is 6-13.8 parts.
Further, in preferred embodiments of the present invention, modifying agent includes diatomite, white carbon, the acyl of cyanuric acid one
Amine, ammeline, melamine polyphosphate, silane coupler, AEO, 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%th, ammelide 1-10%, ammeline 10-45%, silane coupler 0.05-5%.
Further, in preferred embodiments of the present invention, ammonia concn is 0.5%-10%.
Further, in preferred embodiments of the present invention, ammonia concn is 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, comprises the following steps：By melamine, trimerization
Cyanic acid, modifying agent and ammoniacal liquor are mixed to form mixture by weight；In temperature it is 90-110 DEG C by mixture, pressure is
0.1-1Mpa, mixing speed obtains slurry to react 0.5-2.5h under conditions of 100-400r/min；Slurry is subjected to spraying dry
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 that the present invention is provided and preparation method thereof is：
(1) high-performance melamine cyanurate provided in an embodiment of the present invention, its raw material includes melamine, melamine
Acid, modifying agent and ammoniacal liquor；In embodiments of the present invention, the melamine of use, cyanuric acid are technical grade, melamine matter
Measure degree 99.8%, cyanuric acid mass percentage content 98.5%；
Wherein, it is white single under a kind of azacyclo- organic compound produced by raw material of urea, normal temperature that melamine, which is,
Oblique Crystal, without notable 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, available for synthesis chlorinated derivative, sym-closene；Sodium dichloro cyanurate or potassium；For closing
Into 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 aid in controlling the particle diameter of melamine cyanurate, so that
Prepare that a kind of viscosity is relatively low, more flowability, the preferable slurry of mechanical property；
In embodiments of the present invention, modifying agent preferably includes diatomite, white carbon, ammelide, cyanuric acid
Diamides, melamine polyphosphate, silane coupler, AEO, polyoxyethylene carboxylate, polyoxyethylene
At least two in Arlacel-80；In the present embodiment, in order to further reduce the viscosity of slurry, slurry is improved
Mobility, preferably, by mass percentage, modifying agent include diatomite 30-50%, ammelide 1-
10%th, ammeline 10-45%, silane coupler 0.05-5%, the ratio range are tried by inventor's creativeness
Test and obtain, in the ratio range, between each modifying agent raw material can Synergistic, further prepare viscosity it is low, flowing
The good slurry of property.
Ammoniacal liquor, in embodiments of the present invention, reaction medium is used as using ammonia spirit, it is possible to increase melamine cyanurate
The yield and purity of salt, obtain product granularity uniformly, purity is higher, and solids 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
Count by weight, including 100-110 parts of melamine, 100-110 parts of cyanuric acid, 3-15 parts of modifying agent and ammoniacal liquor 350-
800 parts ", the ratio range is obtained by inventor's creativeness experiment, in the ratio range, can be carried out between each raw material
Farthest react, reduce the waste of raw material, the production of melamine cyanurate is carried out using the ratio, enable to production
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 enter one
The viscosity of step reduction slurry, the mobility for improving slurry；And solid accounts for the mass percent of solid-liquid summation for 25-33% ", solid
The viscosity of reduction generation slurry can be aided in by accounting for the mass percent of solid-liquid summation；In embodiments of the present invention, ammonia concn is
0.5%-10%, the ammoniacal liquor in the concentration range can further improve the yield and purity of melamine cyanurate, excellent
Selection of land, when ammonia concn is 0.5%-10%, the yield and purity of the melamine cyanurate prepared are optimal.
(3) preparation method of high-performance melamine cyanurate provided in an embodiment of the present invention, the preparation method includes：
Melamine, cyanuric acid, modifying agent and ammoniacal liquor are first mixed to form mixture by weight；It is in temperature by mixture again
90-110 DEG C, pressure be that 0.1-1MPa, mixing speed are to react 0.5-2.5h under conditions of 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, and this is higher
Solids content obtain easily prepared process conditions, and obtained by the selection of raw material and the proportioning collective effect of each raw material；Then
Slurry is directly spray-dried and cyclonic separation, high-performance melamine cyanurate product is made, it is necessary to illustrate,
In embodiments of the present invention, the granularity of the high-performance melamine cyanurate prepared is D50=0.6-1.5 μm, D98
=1.8-3.5 μm, this production technology for having benefited from use of the embodiment of the present invention can be avoided during conventional size reduction to melamine
The destruction that amine cyanurate crystal is caused, the granularity of obtained melamine cyanurate is excellent；In view of environmental protection, do not make
Into environmental pollution, it is preferable that in embodiments of the present invention, then to tail gas through washing, qualified discharge after pickling；Water lotion is supplemented
Part ammonia is reused, and the concentrated crystallizing and drying of pickle obtains ammonium salt.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
Embodiment 1
A kind of high-performance melamine cyanurate, its raw materials by weight portion meter, including 100 parts of melamine, trimerization
(modifying agent is constituted for 103 parts of cyanic acid, modifying agent：Diatomite 44.5%, ammelide 10%, ammeline
45%th, 3- aminopropyltriethoxies diethoxy silane 0.5%) 3 parts and 800 parts of ammoniacal liquor.
A kind of preparation method of high-performance melamine cyanurate, comprises the following steps：
100 parts of 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 ammoniacal liquor is added in low pressure reaction kettle, stirring at low speed is opened, the material after mixing is slowly added to from charge door
Reactor；Material accounts for the 20.4% of raw material summation；Add after material, close charge door, be warming up to 90 DEG C, control pressure 0.1MPa,
Mixing speed rises to 100r/min, reacts 0.5h, forms slurry；Slurry is released, its grain graininess and solids content is surveyed, 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 composition and granularity of cyanurate, test result are shown in Table 1.
Embodiment 2
A kind of high-performance melamine cyanurate, its raw materials by weight portion meter, including 110 parts of melamine, trimerization
(modifying agent is constituted for 115 parts of cyanic acid, modifying agent：Diatomite 40%, ammelide 10%, ammeline 45%,
3- aminopropyltriethoxies diethoxy silane 5%) 15 parts and 450 parts of ammoniacal liquor.
A kind of preparation method of high-performance melamine cyanurate, comprises the following steps：
110 parts of 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 ammoniacal liquor is added in low pressure reaction kettle, stirring at low speed is opened, the material after mixing is slowly added to from charge door
Reactor；Material accounts for the 34.8% of raw material summation；Add after material, close charge door, be warming up to 90 DEG C, control pressure 0.1MPa,
Mixing speed rises to 200r/min, reacts 2h, forms slurry；Slurry is released, its grain graininess and solids content, test knot is 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 composition and granularity of lithate, test result are shown in Table 1.
Embodiment 3
A kind of high-performance melamine cyanurate, its raw materials by weight portion meter, including 105 parts of melamine, trimerization
(modifying agent is constituted for 110 parts of cyanic acid, modifying agent：Diatomite 44%, ammelide 10%, ammeline 45%,
3- aminopropyltriethoxies diethoxy silane 1%) 13.8 parts and 465 parts of ammoniacal liquor.
A kind of preparation method of high-performance melamine cyanurate, comprises the following steps：
105 parts of 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 ammoniacal liquor；First ammoniacal liquor is added in low pressure reaction kettle, stirring at low speed is opened, the material after mixing is slowly added from charge door
Enter reactor；Material accounts for the 33.0% of raw material summation；Add after material, close charge door, be warming up to 90 DEG C, control pressure
0.1MPa, mixing speed rises to 300r/min, reacts 2.5h, forms slurry；Slurry is released, its grain graininess is surveyed and solid contains
Amount, test result is shown in Table 1；Again by slurry is spray-dried and cyclonic separation, melamine cyanurate product is obtained；Survey gained three
The composition and granularity of poly cyanamid cyanurate, test result are shown in Table 1.
Embodiment 4
A kind of high-performance melamine cyanurate, its raw materials by weight portion meter, including 115 parts of melamine, trimerization
(modifying agent is constituted for 120 parts of cyanic acid, modifying agent：Diatomite 44.5%, ammelide 10%, ammeline
45%th, 3- aminopropyltriethoxies diethoxy silane 0.5%) 10 parts and 600 parts of ammoniacal liquor.
A kind of preparation method of high-performance melamine cyanurate, comprises the following steps：
115 parts of 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 ammoniacal liquor is added in low pressure reaction kettle, stirring at low speed is opened, the material after mixing is slowly added to from charge door
Reactor；Material accounts for the 29.0% of raw material summation；Add after material, close charge door, be warming up to 95 DEG C, control pressure 0.3MPa,
Mixing speed rises to 300r/min, reacts 2.0h, forms slurry；Slurry is released, its grain graininess and solids content is surveyed, 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 composition and granularity of cyanurate, test result are shown in Table 1.
Comparative example 1
Melamine cyanurate prepared by traditional handicraft：Its raw materials by weight portion meter, including 50 parts of melamine,
50 parts of cyanuric acid, 900 parts of water.
The preparation method of melamine cyanurate prepared by traditional handicraft：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, adds 100 parts of melamines, is warming up to 100 DEG C, stirring reaction
4h, generates the slurry of melamine cyanurate, slurry is released, its grain graininess and solids content is surveyed, test result is shown in Table
1；Slurry is filtered successively, dried, acquisition melamine cyanurate product is crushed.Survey gained melamine cyanurate into
Divide and granularity, test result is shown in Table 1.
Comparative example 2
Melamine cyanurate prepared by ammonia-water systems：Its raw materials by weight portion meter, including 100 parts of melamine,
103 parts of cyanuric acid, 800 parts of ammoniacal liquor.
The preparation method of melamine cyanurate prepared by ammonia-water systems：800 part of 5% ammonia is first added in a kettle.
Water, then adds 103 parts of cyanuric acids, and stirring is warming up to 90 DEG C or so, adds 100 parts of melamines, is warming up to 95 DEG C, stirring
2h is reacted, the slurry of melamine cyanurate is generated, slurry is released, its grain graininess and solids content, test result is surveyed
It is shown in Table 1；Slurry is filtered successively, dried, acquisition melamine cyanurate product is crushed.Survey gained melamine cyanurate
Composition and granularity, test result is shown in Table 1.
The embodiment 1-5 of table 1 and comparative example 1-2 slurry property and melamine cyanurate property contrast
The result shows that the raw material components and preparation technology of melamine cyanurate provided by the present invention are prepared
The purity of melamine cyanurate, dispersiveness 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 then added to double-screw injection molding added to after mixing in 94 parts of PA6 with after extruding pelletizing, drying in double screw extruder
In machine, melting blending is molded into standard specimen, and performance detection is carried out respectively to it, wherein, tensile strength (MPa) is used
ISO527~2, elongation at break (%) uses ISO527~2, and flame retardant rating uses UL94 testing vertical flammabilities, testing result
It is shown in Table 2.
The application performance contrast of melamine cyanurate prepared by the 1-4 of the embodiment of the present invention of table 2 and comparative example 1-2
The melamine cyanurea prepared in ratio range using formula provided in an embodiment of the present invention and each component
Hydrochlorate, good with heat endurance, flame retarding efficiency is high, good dispersion, the advantage such as combination property is excellent；This prepares melamine cyanurate
The method of salt, production efficiency is high, with short production cycle, and preparation process is simple, the product mechanical property and fire resistance prepared
It is splendid.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of high-performance melamine cyanurate, it is characterized in that：It is made up, the raw materials by weight portion meter, wraps of raw material
Include 350-800 parts of 100-110 parts of melamine, 100-110 parts of cyanuric acid, 3-15 parts of modifying agent and ammoniacal liquor.
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：Count 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 modifying agent includes diatom
Soil, white carbon, ammelide, ammeline, melamine polyphosphate, silane coupler, poly alkyl alcohol
At least two in oxygen vinethene, polyoxyethylene carboxylate, polyoxyethylene sorbitan monooleate.
5. high-performance melamine cyanurate according to claim 4, it is characterized in that：By mass percentage, it is described
Modifying agent includes diatomite 30-50%, ammelide 1-10%, ammeline 10-45%, silane coupler
0.05-5%.
6. high-performance melamine cyanurate according to claim 1, it is characterized in that：The ammonia concn is 0.5%-
10%.
7. high-performance melamine cyanurate according to claim 6, it is characterized in that：The ammonia concn is 2%-
7%.
8. 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.
9. a kind of preparation method of high-performance melamine cyanurate as described in claim 1-8 any one, its feature
It is：Comprise the following steps：
Melamine, cyanuric acid, modifying agent and ammoniacal liquor are mixed to form mixture by the parts by weight；By the mixture
Temperature be 90-110 DEG C, pressure be that 0.1-1MPa, mixing speed are to react 0.5-2.5h under conditions of 100-400r/min, obtain
To slurry；The slurry is spray-dried and cyclonic separation.
10. the preparation method of high-performance melamine cyanurate according to claim 9, it is characterized in that：By quality hundred
Divide than counting, the content of solid is 20-35% in the slurry.
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| RU2758252C1 (en) * | 2021-03-15 | 2021-10-27 | Федеральное государственное автономное образовательное учреждение высшего образования «Национальный исследовательский Томский государственный университет» | Method for obtaining melamine cyanurate |
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