CN106366104B - Inorganic hybridization polyalcohol etherificate melmac and preparation method thereof - Google Patents
Inorganic hybridization polyalcohol etherificate melmac and preparation method thereof Download PDFInfo
- Publication number
- CN106366104B CN106366104B CN201610623946.2A CN201610623946A CN106366104B CN 106366104 B CN106366104 B CN 106366104B CN 201610623946 A CN201610623946 A CN 201610623946A CN 106366104 B CN106366104 B CN 106366104B
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- Prior art keywords
- polyalcohol
- inorganic hybridization
- melmac
- reaction
- etherificate
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- 150000005846 sugar alcohols Polymers 0.000 title claims abstract description 57
- 238000009396 hybridization Methods 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 238000006266 etherification reaction Methods 0.000 claims abstract description 13
- 239000003973 paint Substances 0.000 claims abstract description 13
- YGCOKJWKWLYHTG-UHFFFAOYSA-N [[4,6-bis[bis(hydroxymethyl)amino]-1,3,5-triazin-2-yl]-(hydroxymethyl)amino]methanol Chemical compound OCN(CO)C1=NC(N(CO)CO)=NC(N(CO)CO)=N1 YGCOKJWKWLYHTG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052796 boron Inorganic materials 0.000 claims abstract description 11
- 229920000570 polyether Polymers 0.000 claims abstract description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims abstract description 8
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 62
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 14
- 229920000877 Melamine resin Polymers 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004814 polyurethane Substances 0.000 claims description 7
- 229920002635 polyurethane Polymers 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 6
- 229920005830 Polyurethane Foam Polymers 0.000 claims description 5
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 5
- 239000011496 polyurethane foam Substances 0.000 claims description 5
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims description 4
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical compound O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 150000002009 diols Chemical class 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 229920000180 alkyd Polymers 0.000 claims description 2
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 2
- YZYDPPZYDIRSJT-UHFFFAOYSA-K boron phosphate Chemical compound [B+3].[O-]P([O-])([O-])=O YZYDPPZYDIRSJT-UHFFFAOYSA-K 0.000 claims description 2
- 229910000149 boron phosphate Inorganic materials 0.000 claims description 2
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- -1 ethyl-butyl Chemical group 0.000 claims description 2
- 239000006260 foam Substances 0.000 claims description 2
- 229940051250 hexylene glycol Drugs 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 claims description 2
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 2
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 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 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 6
- 239000011733 molybdenum Substances 0.000 abstract description 6
- 229920003180 amino resin Polymers 0.000 abstract description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract 1
- 229920001721 polyimide Polymers 0.000 description 7
- 239000009719 polyimide resin Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 239000004640 Melamine resin Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005829 trimerization reaction Methods 0.000 description 2
- 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 description 1
- UVHLUYZMNUCVJN-UHFFFAOYSA-N 3-methyloctane-4,4-diol Chemical compound CCCCC(O)(O)C(C)CC UVHLUYZMNUCVJN-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 229920003270 Cymel® Polymers 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- WJEIYVAPNMUNIU-UHFFFAOYSA-N [Na].OC(O)=O Chemical compound [Na].OC(O)=O WJEIYVAPNMUNIU-UHFFFAOYSA-N 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3897—Low-molecular-weight compounds having heteroatoms other than oxygen containing heteroatoms other than oxygen, halogens, nitrogen, sulfur, phosphorus or silicon
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Polyethers (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention belongs to inorganic hybridization technical field of polymer materials, more particularly to a kind of inorganic hybridization polyalcohol etherificate melmac and preparation method thereof.Mainly include the following steps that：(1) etherification reaction, hexamethylolmelamine is added into reaction kettle and polyalcohol carries out insulation reaction, obtains four etherificates or five etherificate melmacs；(2) alkali neutralization；(3) hydridization is reacted；(4) distillation removes remaining polyalcohol；(5) cold filtration obtains finished product.Melmac is etherified by inorganic hybridization polyalcohol made from method of the present invention, pass through the hybrid cross-linked reaction with inorganic hybridization compound, so that the amino resins polyalcohol ultimately generated introduces the heat-resistant fireproof element such as boron, molybdenum, antimony, so as to improve the resistance to elevated temperatures and fire resistance of amino resins polyalcohol, it is mainly used in and prepares combined polyether and paint.
Description
Technical field
The invention belongs to inorganic hybridization technical field of polymer materials, more particularly to a kind of inorganic hybridization polyalcohol etherificate three
Cymel with and preparation method thereof.
Background technology
Since amino resins has certain heat resistance, so in many fields, including coating industry, furniture industry,
Polyurethane industries among others etc. have application.But applied on the polyurethane material of high fire-retardance, its resistance to elevated temperatures still has certain
Gap.
Due to the special construction of polyurethane foam plastics molecule, its easily burning, characteristic of non-refractory is determined.With
The continuous popularization and application of polyurethane energy-saving heat preserving hard bubble application technology, the requirement to its fire resistance is also higher and higher, particularly
GB8624-2012《Classification on burning behaviour for building materials》And GB50016-2014《Code for fire protection design of buildings》Promulgation it is real
Shi Hou, polyurethane foam are conveniently faced with acid test in fire retardant performance.Therefore, the resistance to height of amino resins how is improved
Gentle fire resistance is into urgent technical problem to be solved in the field.
The content of the invention
In order to solve the above problem existing in the prior art, the present invention provides a kind of inorganic hybridization polyalcohol to be etherified trimerization
Melamine resin and preparation method thereof, using hexamethylolmelamine as raw material, under the conditions of acid medium, gives birth to polyol reaction
Reacted, generated into tetramethyl etherified melamine polyimide resin or five methyl-etherified melmacs, then with inorganic hybridization compound
Inorganic hybridization polyalcohol is etherified melmac, has higher fire resistance and resistance to elevated temperatures.
The technical solution adopted in the present invention is as follows：
Inorganic hybridization polyalcohol is etherified melmac, it is characterised in that：Molecular structure is as follows：
X in the molecular structure is one kind in inorganic hybridization element, including B or Sb；
R in the molecular structure is-(CH2)nOH or-(CH2)mO(CH2)mOH or-(OCH2CH2CH2CH3)KOH
Or-O (CH2)PCH(OH)CH2OH or-OCH2C(CH2OH)3, wherein 2≤n≤6,2≤m≤6,2≤p≤6,2≤k≤41.
The preparation method of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：It is main include with
Lower step：
Under the conditions of acid medium, the polyalcohol that the R in hexamethylolmelamine and claim 1 is represented carries out ether
Change reaction and obtain polyalcohol etherificate melmac, under agitation plus alkali carries out alkali neutralization reaction；
It is small that the melmac of etherificate is reacted under conditions of 100~110 DEG C with inorganic hybridization compound to 0.5-2
When, hydridization reaction is completed, and is cooled to 60-80 DEG C, salt is filtered out with filter, obtains inorganic hybridization polyalcohol etherificate melamine
Resin.
The preparation method of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：It is main include with
Lower specific steps：
(1) etherification reaction
The polyalcohol that the R added into reaction kettle in hexamethylolmelamine and claim 1 is represented, adds acid for adjusting pH
For 2.5~5.5, under conditions of 35~65 DEG C, mixing speed is 60~80 revs/min, and 30~120min of insulation is etherified
Reaction, obtains polyalcohol etherificate melmac；
(2) alkali neutralization
It is stirred under the conditions of 40-80 revs/min of rotating speed, it is 8.0~9.0 to add alkali to adjust pH, which protects
Temperature is held less than 50 DEG C；
(3) hydridization is reacted
Inorganic hybridization compound and water are added into reaction kettle, be warming up to 100-110 DEG C of reaction 0.5-2 it is small when, hydridization is anti-
It should complete；
(4) distillation removes remaining polyalcohol
Under conditions of vacuum 0.090-0.1MPa, 100-130 DEG C of temperature, the remaining of the middle addition of step (1) is steamed
Polyalcohol；
(5) cold filtration
60-80 DEG C is cooled to, 2%~2.5% super-cell is added, filters out salt with filter, obtain inorganic miscellaneous
Change polyalcohol etherificate melmac.
The preparation method of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：The step (3)
In inorganic hybridization compound be：Boratex, potassium borate, boric acid, zinc borate, boron phosphate, four water, eight Boratex, three oxidations two
One kind in antimony, antimony pentoxide, sodium molybdate, potassium molybdate, zinc molybdate, ammonium molybdate, ammonium tetramolybdate or ammonium heptamolybdate.
The preparation method of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：The step (1)
Or acid used in adjusting pH is hydrochloric acid or nitric acid in step (2), its mass concentration is 31-36%, and alkali used is sodium hydroxide, carbonic acid
Sodium, sodium acid carbonate, potassium hydroxide or potassium carbonate, its mass concentration are 25-35%.
The preparation method of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：The step (1)
In polyalcohol for propane diols, ethylene glycol, diethylene glycol, dipropylene glycol, butanediol, hexylene glycol, ethyl butyl propanediol, poly- four
One kind in hydrogen furans glycol, glycerine or pentaerythrite.
The application of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：The inorganic hybridization is more
The etherified melmac of member is used to prepare combined polyether, and the combined polyether includes use for hard bubble of polyurethane combined polyether, gathers
Half hard bubble combined polyether of urethane, soft polyurethane foam combined polyether.
The application of the inorganic hybridization polyalcohol etherificate melmac, it is characterised in that：The inorganic hybridization is more
The etherified melmac of member is used to prepare paint, and the paint includes alkyd paint coating, high concentrations of toluene diisocyanate
Coating, epoxy resin paint coating, acrylic paint coating, amino paint.
The inorganic hybridization reaction principle of patent of the present invention：
The principle of reaction can be crosslinked with boron, molybdenum, antimony element using the methylol contained in compound, realizes this hair
The hydridization reaction process of bright patent, because enclosing methylol, eliminates reactive group, and the temperature in reaction process can be significantly
Degree improves and boron, molybdenum, antimony ignition-proof element is introduced to 110 DEG C, and on molecular structure so that stability, the fire resistance of product
It is substantially improved with resistance to elevated temperatures.
The above-mentioned technical proposal of the present invention compared with prior art, has the following advantages：
1st, the melmac by etherificate and the hybrid cross-linked reaction of inorganic hybridization compound so that ultimately generate
Melmac polyalcohol introduces the heat-resistant fireproof element such as boron, antimony, molybdenum, so as to improve the resistance to of amino resins polyalcohol
High-temperature behavior and fire resistance, compared with the resin before non-hydridization, resistance to elevated temperatures improves more than 50 DEG C, and fire resistance improves
At least 20%.
2nd, the preparation of inorganic hybridization polyalcohol etherificate melmac overcomes polyalcohol etherificate melmac
Molecular structure introduces the technical barrier of ignition-proof element, solves influence and resistance of the outer addition fire retardant to product physical mechanical property
The technical problems such as fuel efficiency fruit is undesirable.
3rd, heat-resistant fireproof melmac polyalcohol is prepared into this heat-resistant fireproof melmac, with isocyanide
Acid esters MDI reacts, the inorganic hybridization polyurethane with melamine foamed material excellent physical properties of formation, and intensity is high, not hair powder, no
Modification, is fully achieved that GB50404-2007 standards are waterproof thermal-insulated and the B1 grades of fire-retardant requirements of GB8624-2012 standards.Ensureing thing
While rationality energy, excellent fireproof performance, its oxygen index (OI) is more than 30%.
4th, since prepared melmac polyalcohol has high flame resistance and resistance to elevated temperatures, thus with its
When producing polyurethane foam, it is not necessary to expensive high fire-retardance phosphate flame retardant is used, makes the reduction of foam cost greatly,
More than 30% is reduced, economy is more reasonable.
Embodiment
With reference to specific embodiment, the present invention will be described in detail, but the invention is not limited in specific embodiment.
Embodiment 1
Boron hydridization propane diols is etherified the preparation of melmac
Molecular structural formula：
Raw material proportioning：
(1) etherification reaction
Hexamethylolmelamine and propane diols are added in reaction kettle according to the above ratio, it is 2.5 to add acid for adjusting pH, 35
Under conditions of DEG C, mixing speed carries out etherification reaction for 60 revs/min of insulation 120min, obtains propane diols etherificate melamine tree
Fat；
(2) alkali neutralization
It is stirred under the conditions of 40 revs/min of rotating speed, it is 8.0 to add alkali to adjust pH, which keeps temperature low
In 50 DEG C；
(3) hydridization is reacted
Four water, eight Boratex and water are added into reaction kettle, be warming up to 100 DEG C reaction 2 it is small when, hydridization reaction complete；
(4) distillation removes remaining polyalcohol
Under conditions of vacuum 0.090MPa, 130 DEG C of temperature, the remaining propane diols added in step (1) is steamed；
(5) cold filtration
60 DEG C are cooled to, 2% super-cell is added, salt is filtered out with filter, obtains boron hydridization propane diols etherificate
Melmac, yield 99.0%.
Embodiment 2
Stilba diethylene glycol is etherified the preparation of melmac
Molecular structural formula：
Raw material proportioning：
(1) etherification reaction
Hexamethylolmelamine and diethylene glycol are added in reaction kettle according to the above ratio, it is 5.5 to add acid for adjusting pH,
Under conditions of 65 DEG C, mixing speed is 80 revs/min, and insulation 30min carries out etherification reaction, obtains diethylene glycol etherificate melamine
Polyimide resin；
(2) alkali neutralization
It is stirred under the conditions of 80 revs/min of rotating speed, it is 9.0 to add alkali to adjust pH, which keeps temperature low
In 50 DEG C；
(3) hydridization is reacted
Antimony oxide and water are added into reaction kettle, be warming up to 110 DEG C of reactions 0.5 it is small when, hydridization reaction is completed；
(4) distillation removes remaining polyalcohol
Under conditions of vacuum 0.1MPa, 100 DEG C of temperature, the remaining diethylene glycol added in step (1) is steamed；
(5) cold filtration
80 DEG C are cooled to, 2.5% super-cell is added, filters out salt with filter, obtain stilba diethylene glycol
Etherified melamine polyimide resin, yield 98.5%.
Embodiment 3
The preparation of boron hydridization polytetrahydrofuran diol etherified melamine polyimide resin
Molecular structural formula：
Raw material proportioning：
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added in reaction kettle according to the above ratio, add the acid for adjusting pH to be
3.5, under conditions of 45 DEG C, mixing speed is 70 revs/min, and insulation 50min carries out etherification reaction, obtains PolyTHF two
Etherified melmac；
(2) alkali neutralization
It is stirred under the conditions of 50 revs/min of rotating speed, it is 8.2 to add alkali to adjust pH, which keeps temperature low
In 50 DEG C；
(3) hydridization is reacted
Four water, eight Boratex and water are added into reaction kettle, be warming up to 105 DEG C reaction 1 it is small when, hydridization reaction complete；
(4) distillation removes remaining polyalcohol
Under conditions of vacuum 0.090MPa, 110 DEG C of temperature, the remaining poly- tetrahydrochysene furan added in step (1) is steamed
Mutter glycol；
(5) cold filtration
70 DEG C are cooled to, 2% super-cell is added, filters out salt with filter, obtain boron hydridization PolyTHF
Glycol is etherified melmac, yield 98.1%.
Embodiment 4
The preparation of molybdenum hydridization glycerine etherified melamine polyimide resin
Molecular structural formula：
Raw material proportioning：
(1) etherification reaction
Hexamethylolmelamine and glycerine are added in reaction kettle according to the above ratio, it is 4.5 to add acid for adjusting pH, 40
Under conditions of DEG C, mixing speed is 65 revs/min, and insulation 90min carries out etherification reaction, obtains glycerine etherified melamine amine tree
Fat；
(2) alkali neutralization
It is stirred under the conditions of 70 revs/min of rotating speed, it is 8.5 to add alkali to adjust pH, which keeps temperature low
In 50 DEG C；
(3) hydridization is reacted
Sodium molybdate and water are added into reaction kettle, be warming up to 105 DEG C of reactions 1.5 it is small when, hydridization reaction is completed；
(4) distillation removes remaining polyalcohol
Under conditions of vacuum 0.1MPa, 120 DEG C of temperature, the remaining glycerine added in step (1) is steamed；
(5) cold filtration
75 DEG C are cooled to, 2% super-cell is added, salt is filtered out with filter, obtains molybdenum hydridization glycerine etherificate
Melmac, yield 98.2%.
Embodiment 5
The preparation of boron hydridization pentaerythrite etherified melamine polyimide resin
Molecular structural formula：
Raw material proportioning：
(1) etherification reaction
Hexamethylolmelamine and pentaerythrite are added in reaction kettle according to the above ratio, it is 4.0 to add acid for adjusting pH,
Under conditions of 60 DEG C, mixing speed is 65 revs/min, and insulation 110min carries out etherification reaction, obtains pentaerythrite etherificate trimerization
Melamine resin；
(2) alkali neutralization
It is stirred under the conditions of 50 revs/min of rotating speed, it is 8.6 to add alkali to adjust pH, which keeps temperature low
In 50 DEG C；
(3) hydridization is reacted
Boratex and water are added into reaction kettle, be warming up to 102 DEG C of reactions 1.5 it is small when, hydridization reaction is completed；
(4) distillation removes remaining polyalcohol
Under conditions of vacuum 0.1MPa, 120 DEG C of temperature, the remaining pentaerythrite added in step (1) is steamed；
(5) cold filtration
60 DEG C are cooled to, 2.5% super-cell is added, filters out salt with filter, obtain inorganic hybridization polyalcohol
Etherified melamine polyimide resin, yield 98.0%.
Claims (8)
1. inorganic hybridization polyalcohol is etherified melmac, it is characterised in that：Molecular structure is as follows：
X in the molecular structure is inorganic hybridization element, one kind in B or Sb；
R in the molecular structure is-(CH2)nOH or-(CH2)mO(CH2)mOH or
- (OCH2CH2CH2CH3)KOH or-O (CH2)PCH(OH)CH2OH or-OCH2C(CH2OH)3, wherein 2≤n≤6,2≤m
≤ 6,2≤p≤6,2≤k≤41.
2. the preparation method of inorganic hybridization polyalcohol etherificate melmac as claimed in claim 1, it is characterised in that：It is main
Comprise the following steps：
Under the conditions of acid medium, the polyalcohols represented of the R in hexamethylolmelamine and claim 1 be etherified anti-
Polyalcohol etherificate melmac should be obtained, under agitation plus alkali carries out alkali neutralization reaction；
It is miscellaneous by the melmac of etherificate and inorganic hybridization compound when reaction 0.5~2 is small under conditions of 100~110 DEG C
Change reaction to complete, be cooled to 60~80 DEG C, salt is filtered out with filter, obtain inorganic hybridization polyalcohol etherificate melamine tree
Fat.
3. the preparation method of inorganic hybridization polyalcohol etherificate melmac as claimed in claim 2, it is characterised in that：It is main
To include step in detail below：
(1) etherification reaction
The polyalcohol that the R added into reaction kettle in hexamethylolmelamine and claim 1 is represented, adds the acid for adjusting pH to be
2.5~5.5, under conditions of 35~65 DEG C, mixing speed is 60~80 revs/min, and 30~120min of insulation be etherified anti-
Should, obtain polyalcohol etherificate melmac；
(2) alkali neutralization
It is stirred under the conditions of 40~80 revs/min of rotating speed, it is 8.0~9.0 to add alkali to adjust pH, which keeps temperature
Degree is less than 50 DEG C；
(3) hydridization is reacted
Inorganic hybridization compound and water are added into reaction kettle, be warming up to 100~110 DEG C of reactions 0.5~2 it is small when, hydridization reaction
Complete；
(4) distillation removes remaining polyalcohol
Under conditions of 0.090~0.1MPa of vacuum, 100~130 DEG C of temperature, steam add in step (1) it is remaining more
First alcohol；
(5) cold filtration
60~80 DEG C are cooled to, 2%~2.5% super-cell is added, filters out salt with filter, it is more to obtain inorganic hybridization
The etherified melmac of member.
4. the preparation method of inorganic hybridization polyalcohol etherificate melmac according to claim 3, it is characterised in that：
Inorganic hybridization compound in the step (3) is：Boratex, potassium borate, boric acid, zinc borate, boron phosphate, four water, eight boric acid
One in sodium, antimony oxide, antimony pentoxide, sodium molybdate, potassium molybdate, zinc molybdate, ammonium molybdate, ammonium tetramolybdate or ammonium heptamolybdate
Kind.
5. the preparation method of inorganic hybridization polyalcohol etherificate melmac according to claim 3, it is characterised in that：
Acid used in adjusting pH in the step (1) or step (2) is hydrochloric acid or nitric acid, its mass concentration is 31~36%, and alkali used is
Sodium hydroxide, sodium carbonate, sodium acid carbonate, potassium hydroxide or potassium carbonate, its mass concentration are 25~35%.
6. the preparation method of inorganic hybridization polyalcohol etherificate melmac according to claim 3, it is characterised in that：
Polyalcohol in the step (1) is propane diols, ethylene glycol, diethylene glycol, dipropylene glycol, butanediol, hexylene glycol, ethyl-butyl
One kind in propane diols, polytetrahydrofuran diol, glycerine or pentaerythrite.
7. the application of inorganic hybridization polyalcohol etherificate melmac according to claim 1, it is characterised in that：It is described
Inorganic hybridization polyalcohol etherificate melmac is used to prepare combined polyether, and the combined polyether includes use for hard bubble of polyurethane group
Polyethers, polyurethane semihard foam are closed with combined polyether, soft polyurethane foam combined polyether.
8. the application of inorganic hybridization polyalcohol etherificate melmac according to claim 1, it is characterised in that：It is described
Inorganic hybridization polyalcohol etherificate melmac is used to prepare paint, the paint include alkyd paint coating,
High concentrations of toluene diisocyanate coating, epoxy resin paint coating, acrylic paint coating, amino paint.
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| CN201610623946.2A CN106366104B (en) | 2016-08-01 | 2016-08-01 | Inorganic hybridization polyalcohol etherificate melmac and preparation method thereof |
| PCT/CN2017/078237 WO2018023984A1 (en) | 2016-08-01 | 2017-03-26 | Inorganic hybrid polyol etherified melamine resin and preparation method therefor |
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