CN106188522B - Inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin and preparation method thereof - Google Patents
Inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin and preparation method thereof Download PDFInfo
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- CN106188522B CN106188522B CN201610619441.9A CN201610619441A CN106188522B CN 106188522 B CN106188522 B CN 106188522B CN 201610619441 A CN201610619441 A CN 201610619441A CN 106188522 B CN106188522 B CN 106188522B
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/338—Polymers modified by chemical after-treatment with inorganic and organic compounds
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5021—Polyethers having heteroatoms other than oxygen having nitrogen
- C08G18/5054—Polyethers having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/12—Polyurethanes from compounds containing nitrogen and active hydrogen, the nitrogen atom not being part of an isocyanate group
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterized by the type of post-polymerisation functionalisation
- C08G2650/04—End-capping
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- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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Abstract
The invention belongs to inorganic hybridization technical field of polymer materials, in particular to a kind of inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin and preparation method thereof.It mainly comprises the steps that (1) etherification reaction, hexamethylolmelamine is added into reaction kettle and polytetrahydrofuran diol carries out insulation reaction, obtain four etherificates or five etherificate melamine resins；(2) alkali neutralization；(3) hydridization is reacted；(4) distillation removes remaining polytetrahydrofuran diol；(5) cold filtration obtains finished product.Inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin made from the method through the invention, by being reacted with the hybrid cross-linked of inorganic hybridization compound, so that the amino resins polytetrahydrofuran diol ultimately generated introduces the heat-resistant fireproofs element such as boron, antimony, to improve the high temperature resistance and flame retardant property of amino resins polytetrahydrofuran diol, 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, in particular to a kind of inorganic hybridization polytetrahydrofuran two
Etherified melamine resin with and preparation method thereof.
Background technique
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, high temperature resistance still has centainly
Gap.
Due to the special construction of polyurethane foam plastics molecule, determine that it is easy the characteristic of burning, non-refractory.With
The continuous popularization and application of polyurethane energy-saving heat preserving hard bubble application technology, the requirement to its flame retardant property is also higher and higher, especially
The promulgation of GB8624~2012 " Classification on burning behaviour for building materials " and GB50016~2014 " Code for fire protection design of buildings "
After implementation, polyurethane foam is conveniently faced with acid test in fire retardant performance.Therefore, the resistance to of amino resins how is improved
High temperature and flame retardant property are at urgent technical problem to be solved in the field.
Summary of the invention
In order to solve the above problems existing in the present technology, the present invention provides a kind of inorganic hybridization polytetrahydrofuran diols
Etherified melamine polyimide resin and preparation method thereof, using hexamethylolmelamine as raw material, under the conditions of acid medium, with poly- four
The reaction of hydrogen furans glycol generates tetramethyl etherified melamine polyimide resin or five methyl-etherified melamine resins, then with inorganic hybridization chemical combination
Object is reacted, and inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, flame retardant property with higher and resistance to are generated
High-temperature behavior.
The technical solution adopted in the present invention is as follows:
Inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: molecular structure is as follows:
X in the molecular structure is inorganic hybridization element, including one of B or Sb.
The preparation method of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: main
Want the following steps are included:
Under the conditions of acid medium, hexamethylolmelamine and polytetrahydrofuran diol are subjected to etherification reaction and gathered
Erythritan etherified melamine polyimide resin, under agitation plus alkali carries out alkali neutralization reaction；
It is small that the melamine resin of etherificate with inorganic hybridization compound is reacted 0.5~2 under conditions of 100~110 DEG C
When, hydridization reaction is completed, and is cooled to 60~80 DEG C, is filtered out salt with filter, obtains inorganic hybridization polytetrahydrofuran diol ether
Change melamine resin.
The preparation method of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: main
Want comprising the following specific steps
(1) etherification reaction
The polytetrahydrofuran diol that the R being added in hexamethylolmelamine and claim 1 into reaction kettle is represented, adds
Acid for adjusting pH is 2.5~5.5, and under conditions of 35~65 DEG C, mixing speed is 60~80 revs/min, keeps the temperature 30~120min
Etherification reaction is carried out, polytetrahydrofuran diol etherified melamine polyimide resin is obtained；
(2) alkali neutralization
It is stirred under the conditions of 40~80 revs/min of revolving speed, adding alkali to adjust pH is 8.0~9.0, which protects
Temperature is held lower than 50 DEG C；
(3) hydridization is reacted
Inorganic hybridization compound and water are added into reaction kettle, is warming up to 100~110 DEG C and reacts 0.5~2 hour, hydridization
Reaction is completed；
(4) cold filtration
60~80 DEG C are cooled to, 2%~2.5% super-cell is added, filters out salt with filter, obtains inorganic miscellaneous
Change polytetrahydrofuran diol etherified melamine polyimide resin.
The preparation method of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: institute
State the inorganic hybridization compound in step (3) are as follows: Boratex, potassium borate, boric acid, zinc borate, boron phosphate, four water, eight Boratex,
One of antimony oxide, antimony pentoxide, sodium molybdate, potassium molybdate, zinc molybdate, ammonium molybdate, ammonium tetramolybdate or ammonium heptamolybdate.
The preparation method of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: institute
Stating and adjusting acid used in pH in step (1) or step (2) is hydrochloric acid or nitric acid, and mass concentration is 31~36%, and alkali used is hydrogen
Sodium oxide molybdena, sodium carbonate, sodium bicarbonate, potassium hydroxide or potassium carbonate, mass concentration are 25~35%.
The application of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: the nothing
Machine hydridization polytetrahydrofuran diol etherified melamine polyimide resin is used to prepare combined polyether, and the combined polyether includes rigid polyurethane
Bubble combined polyether, polyurethane semihard foam combined polyether, soft polyurethane foam combined polyether.
The application of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: the nothing
Machine hydridization polytetrahydrofuran diol etherified melamine polyimide resin 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 the invention patent:
The principle reacted can be crosslinked with boron, molybdenum, antimony element using the methylol contained on compound, realize this hair
The hydridization reaction process of bright patent eliminates reactive group because enclosing methylol, and the temperature in reaction process can be substantially
Degree is improved to 110 DEG C, and boron, molybdenum, antimony ignition-proof element are introduced on molecular structure, so that the stability of product, flame retardant property
It is substantially improved with high temperature resistance.
Above-mentioned technical proposal of the invention compared with prior art, has the advantage that
1, it is reacted by the melamine resin of etherificate with the hybrid cross-linked of inorganic hybridization compound, so that ultimately generate
Melamine resin polytetrahydrofuran diol introduces the heat-resistant fireproofs element such as boron, antimony, molybdenum, so that it is poly- to improve amino resins
The high temperature resistance and flame retardant property of erythritan, compared with the resin before non-hydridization, high temperature resistance improves 50 DEG C
More than, flame retardant property improves at least 20%.
2, the preparation of the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin overcomes polytetrahydrofuran diol
Molecular structure introduces the technical problem 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.
3, heat-resistant fireproof polytetrahydrofuran diol ether China melamine is prepared into this heat-resistant fireproof melamine resin
Polyimide resin is reacted with isocyanates MDI, the inorganic hybridization polyurethane with melamine foamed material excellent physical properties of formation, by force
Degree is high, not hair powder, not modification, is fully achieved that the standard of GB50404~2007 is waterproof thermal-insulated and B1 grade of the standard of GB8624~2012 are hindered
The requirement of combustion.While guaranteeing physical property, excellent fireproof performance, oxygen index (OI) is greater than 30%.
4, since prepared melamine resin polytetrahydrofuran diol has high flame resistance and high temperature resistance, institute
Not need to keep foam cost big using expensive high fire-retardance phosphate flame retardant when producing polyurethane foam with it
For reduction, reduce 30% or more, economy is more reasonable.
Specific embodiment
The present invention will be described in detail combined with specific embodiments below, but the invention is not limited to specific embodiments.
Embodiment 1
The preparation of boron hydridization polytetrahydrofuran diol etherified melamine polyimide resin
Molecular structural formula:
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added in reaction kettle, adding 31% salt acid for adjusting pH is 2.5,
Under conditions of 35 DEG C, mixing speed is that 60 revs/min of heat preservation 120min carry out etherification reaction, obtains polytetrahydrofuran diol ether
Change melamine resin；
(2) alkali neutralization
It is stirred under the conditions of 40 revs/min of revolving speed, adding 30% sodium hydroxide adjusting pH is 8.0, the alkali neutralization mistake
Journey keeps temperature to be lower than 50 DEG C；
(3) hydridization is reacted
Four water, eight Boratex and water are added into reaction kettle, is warming up to 100 DEG C and reacts 2 hours, hydridization reaction is completed；
(4) cold filtration
60 DEG C are cooled to, 2% super-cell is added, filters out salt with filter, obtains boron hydridization polytetrahydrofuran
Glycol is etherified melamine resin.
Embodiment 2
The preparation of stilba polytetrahydrofuran diol etherified melamine polyimide resin
Molecular structural formula:
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added in reaction kettle, adding 36% salt acid for adjusting pH is 5.5,
Under conditions of 65 DEG C, mixing speed is 80 revs/min, and heat preservation 30min carries out etherification reaction, obtains polytetrahydrofuran diol ether
Change melamine resin；
(2) alkali neutralization
It is stirred under the conditions of 80 revs/min of revolving speed, adding 30% potassium hydroxide to adjust pH is 9.0, the alkali neutralization process
Temperature is kept to be lower than 50 DEG C；
(3) hydridization is reacted
Antimony oxide and water are added into reaction kettle, is warming up to 110 DEG C and reacts 0.5 hour, hydridization reaction is completed；
(4) cold filtration
80 DEG C are cooled to, 2.5% super-cell is added, filters out salt with filter, obtains the poly- tetrahydro furan of stilbaization
Glycol of muttering is etherified melamine resin.
Embodiment 3
The preparation of molybdenum hydridization polytetrahydrofuran diol etherified melamine polyimide resin
Molecular structural formula:
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added in reaction kettle, adding 31% nitre acid for adjusting pH is 3.5,
Under conditions of 50 DEG C, mixing speed is 60 revs/min, and heat preservation 50min carries out etherification reaction, obtains polytetrahydrofuran diol ether
Change melamine resin；
(2) alkali neutralization
It is stirred under the conditions of 70 revs/min of revolving speed, adding 30% sodium hydroxide to adjust pH is 8.2, the alkali neutralization process
Temperature is kept to be lower than 50 DEG C；
(3) hydridization is reacted
Sodium molybdate and water are added into reaction kettle, is warming up to 105 DEG C and reacts 1.5 hours, hydridization reaction is completed；
(4) cold filtration
70 DEG C are cooled to, 2.5% super-cell is added, filters out salt with filter, obtains the poly- tetrahydro furan of molybdenum hydridization
Glycol of muttering is etherified melamine resin.
Embodiment 4
The preparation of boron hydridization polytetrahydrofuran diol etherified melamine polyimide resin
Molecular structural formula:
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added in reaction kettle, adding 31% nitre acid for adjusting pH is 4.5,
Under conditions of 60 DEG C, mixing speed is 70 revs/min, and heat preservation 110min carries out etherification reaction, obtains polytetrahydrofuran diol
Etherified melamine polyimide resin；
(2) alkali neutralization
It is stirred under the conditions of 75 revs/min of revolving speed, adding 30% sodium bicarbonate to adjust pH is 8.2, the alkali neutralization process
Temperature is kept to be lower than 50 DEG C；
(3) hydridization is reacted
Boratex and water are added into reaction kettle, is warming up to 106 DEG C and reacts 1.0 hours, hydridization reaction is completed；
(4) cold filtration
65 DEG C are cooled to, 2% super-cell is added, filters out salt with filter, obtains boron hydridization polytetrahydrofuran
Glycol is etherified melamine resin.
Embodiment 5
The preparation of molybdenum hydridization polytetrahydrofuran diol etherified melamine polyimide resin
Molecular structural formula:
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added in reaction kettle, adding 31% nitre acid for adjusting pH is 4.5,
Under conditions of 50 DEG C, mixing speed is 70 revs/min, and heat preservation 80min carries out etherification reaction, obtains polytetrahydrofuran diol ether
Change melamine resin；
(2) alkali neutralization
It is stirred under the conditions of 70 revs/min of revolving speed, adding 30% sodium hydroxide to adjust pH is 8.5, the alkali neutralization process
Temperature is kept to be lower than 50 DEG C；
(3) hydridization is reacted
Sodium molybdate and water are added into reaction kettle, is warming up to 105 DEG C and reacts 1 hour, hydridization reaction is completed；
(4) cold filtration
60 DEG C are cooled to, 2.5% super-cell is added, filters out salt with filter, obtains the poly- tetrahydro furan of molybdenum hydridization
Glycol of muttering is etherified melamine resin.
Claims (5)
1. inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin, it is characterised in that: molecular structure is as follows:
Wherein 2≤k≤41；
X in the molecular structure is inorganic hybridization element, is selected from one of B or Sb.
2. the preparation method of inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin as described in claim 1, special
Sign is: mainly comprising the steps that
(1) etherification reaction
Hexamethylolmelamine and polytetrahydrofuran diol are added into reaction kettle, adding acid for adjusting pH is 2.5~5.5,35
Under conditions of~65 DEG C, mixing speed is 60~80 revs/min, and 30~120min of heat preservation carries out etherification reaction, obtains poly- tetrahydro
Furans glycol is etherified melamine resin；
(2) alkali neutralization
It is stirred under the conditions of 40~80 revs/min of revolving speed, adding alkali to adjust pH is 8.0~9.0, which keeps temperature
Degree is lower than 50 DEG C；
(3) hydridization is reacted
Inorganic hybridization compound and water are added into reaction kettle, is warming up to 100~110 DEG C and reacts 0.5~2 hour, hydridization reaction
It completes；
Inorganic hybridization compound in the step (3) are as follows: four water, eight Boratex, antimony oxide, sodium molybdate, in Boratex
It is a kind of；
(4) cold filtration
60~80 DEG C are cooled to, 2%~2.5% super-cell is added, filters out salt with filter, it is poly- to obtain inorganic hybridization
Erythritan etherified melamine polyimide resin.
3. the preparation method of inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin according to claim 2,
Be characterized in that: it is hydrochloric acid or nitric acid that acid used in pH is adjusted in the step (1) or step (2), and mass concentration is 31~36%,
Alkali used is sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide or potassium carbonate, and mass concentration is 25~35%.
4. the application of inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin according to claim 1, feature
Be: the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin is used to prepare combined polyether, the combined polyether
Selected from use for hard bubble of polyurethane combined polyether, polyurethane semihard foam combined polyether, soft polyurethane foam combined polyether.
5. the application of inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin according to claim 1, feature
Be: the inorganic hybridization polytetrahydrofuran diol etherified melamine polyimide resin is used to prepare paint, the paint
Coating, acrylic paint coating, amino paint are painted selected from alkyd paint coating, high concentrations of toluene diisocyanate coating, epoxy resin.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295616A (en) * | 2011-05-18 | 2011-12-28 | 杨彦威 | Amino resin having polyhydroxy structure, and preparation method thereof |
| CN102690661A (en) * | 2012-06-07 | 2012-09-26 | 常州大学 | Hybrid fire retardant and preparing method thereof |
| CN104987484A (en) * | 2015-05-29 | 2015-10-21 | 张家港迪蒙德节能科技有限公司 | Inorganic material hybrid hard melamine polyurethane foam heat insulation material, preparation method thereof and combined polyether used therein |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295616A (en) * | 2011-05-18 | 2011-12-28 | 杨彦威 | Amino resin having polyhydroxy structure, and preparation method thereof |
| CN102690661A (en) * | 2012-06-07 | 2012-09-26 | 常州大学 | Hybrid fire retardant and preparing method thereof |
| CN104987484A (en) * | 2015-05-29 | 2015-10-21 | 张家港迪蒙德节能科技有限公司 | Inorganic material hybrid hard melamine polyurethane foam heat insulation material, preparation method thereof and combined polyether used therein |
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