CN105601858A - Preparation method of amino resin type intumescent flame retardant - Google Patents

Preparation method of amino resin type intumescent flame retardant Download PDF

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Publication number
CN105601858A
CN105601858A CN201610077109.4A CN201610077109A CN105601858A CN 105601858 A CN105601858 A CN 105601858A CN 201610077109 A CN201610077109 A CN 201610077109A CN 105601858 A CN105601858 A CN 105601858A
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melamine
lauxite
pentaerythrite
flame retardant
preparation
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高明
蔡璟路
孙彩云
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North China Institute of Science and Technology
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North China Institute of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
    • C08G12/40—Chemically modified polycondensates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
    • C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
    • C08G12/34—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
    • C08G12/36—Ureas; Thioureas
    • C08G12/38—Ureas; Thioureas and melamines

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)

Abstract

The invention discloses a preparation method of an amino resin type intumescent flame retardant. The preparation method comprises the following steps: (1) synthesis of melamine-urea resin; (2) synthesis of pentaerythritol diphosphate; and (3) synthesis of pentaerythritol diphosphate melamine-urea resin salt. In the preparation method, the pentaerythritol diphosphate prepared in the step (2) is dropwise added into the melamine-urea resin prepared in the step (1) in a stirring state at the mass ratio of 1:(1-2); and after complete addition, the reactions are kept for 10-30min at 60 DEG C to obtain the pentaerythritol diphosphate melamine-urea resin salt which is the amino resin type intumescent flame retardant. According to the method disclosed by the invention, excellent flame retardance of caged bicyclic phosphate can be maintained while the cost can be reduced, influence on the physical properties of the polymer material is little, and moisture absorption is avoided; and since water is used as a solvent in the preparation process, the method conforms to the requirements of environment protection development and has a remarkably broad prospect in application and development.

Description

A kind of preparation method of Amino Resinous Intumescent Flame Retardant
Technical field
The invention belongs to fire proofing technical field, relate to more specifically a kind of Amino Resinous Intumescent Flame RetardantPreparation method.
Background technology
Plastics taking polymer as basic material, rubber, fiber are 20th century emerged and obtained develop rapidlyThree large synthetic materials, have become whole promulgated by the State Council economy, science and technology and military project national defence every field indispensableImportant materials. But most polymer material all belongs to combustible material, easy under the condition such as high temperature, thermal sourceCause fire, cause huge casualties and economic loss. Halogen containing polymers or combine with halogen containing flame-retardantThe flame-retardant polymer forming has good fire resistance, is widely used as fire proofing all the time.But when fire occurs, this class Halogen fire proofing can produce a large amount of smog and poisonous corrosivity halogenationHydrogen, causes into secondary harm. For this reason, European Union in March, 2002 announce " restriction harmful substance refer toMake " regulation, from 1 day July in 2006, all electronic and electrical equipments of selling in European Union member countries can not contain manyThe brominated flame-retardant such as bromo biphenyl and PBDEs, this is restricted the use of halogen-containing flame retardant,Halogen-free flame retardants has become an important trend of fire retardant development. The non-halogen of fire retardant is also fire-retardant workPerson provides a rare research opportunity.
Expanding fire retardant (IFR) is with its distinctive fire retardation and fire retardant mechanism, and low cigarette, low toxicityAdvantage is occupied more and more consequence in flame retardant area, is considered to realize the weight of the non-halogen process of fire retardantWant one of approach. IFR is mainly made up of charcoal source, acid source and source of the gas three parts. Contain this based flame retardantWhen polymer is heated, the acid source catalytic carbon source charing in IFR, source of the gas discharges a large amount of gas makes charring layer swollenSwollen, finally generate one deck uniform carbonaceous froth bed at polymer surfaces, heat insulation, oxygen barrier, press down cigarette, and energyPrevent molten drop, therefore there is good fire resistance, have a extensive future.
At present the good IFR of fire resistance is mainly annular phosphate, particularly taking pentaerythrite as matrixCaged bicyclic phosphate compound is the outstanding person in generally acknowledged expanding fire retardant. From the sixties in last centuryVerkade etc. have synthesized 1-oxygen base phospha-4-methylol-2 first, 6,7-trioxa-l-phosphabicyclo octane (being called for short PEPA)So far,, always by fire-retardant researcher's extensive concern and research, synthesized during this time multiple this compounds, for examplePentaerythritol diphosphate melamine salt (being called for short PDM), two (pentaerythritol phosphate alcohol) melamineAmine phosphate/salt (being called for short Melabis), three (1-oxo-1-phospha-2,6,7-trioxa-l-phosphabicyclo [2.2.2] octanes-4-methylene) phosphate (be called for short Trimer) etc., they are all bicyclo cage shaped taking pentaerythrite as matrixPhosphate, has novel cage structure, and it is highly symmetrical that molecule is, and has abundant charcoal source and acid source concurrently, andAnd excellent heat stability, becomes charcoal good, low toxicity, low cigarette, meet the non-halogen requirement of fire retardant and green ringThe idea of development of protecting, becomes one of study hotspot that flame retardant area is enlivened very much in recent years.
But there is following subject matter in these expanding fire retardants:
(1) building-up process generally adopts the POCl of price comparison costliness3For raw material provides in expanding fire retardantAcid source;
(2) synthetic reaction is at acetonitrile, CH2Cl2And CCl4Carry out Deng in organic solvent, cost is higher, ringEnvironment pollution, complicated operation, post processing trouble;
(3) belong to little molecule fire retardant, easily the moisture absorption;
(4) molecular weight is low, large on the physical property impact of polymeric material itself.
Therefore, cheap, efficient, environmental protection and polymer performance has been affected to little swellable polymer flame-retardant systemBecome an important directions of current flame retardant area development.
Summary of the invention
The object of the invention is to overcome the deficiency of existent technique, provide a kind of amino resins type to expand and hinderThe preparation method of combustion agent.
The present invention is achieved in that a kind of preparation method of Amino Resinous Intumescent Flame Retardant, comprises as followsStep:
Synthesizing of step 1, melamine-Lauxite:
Formalin is joined in container, and regulating pH value with monoethanolamine is 8-10, then according to mol ratio,Formaldehyde: urea: melamine=3-5: 0.2-1: 1, point 3 batches of mixtures by urea and melamine addIn formalin, stir, at 85-95 DEG C, react 1-3 hour, obtain thickness transparence trimerizationCyanamide-Lauxite;
Synthesizing of step 2, pentaerythritol diphosphate:
Taking phosphoric acid and pentaerythrite as initiation material, water, as solvent, stirs, and is warming up to100-140 DEG C is reacted, and the reaction time is 2-5h, separates water outlet, obtains thick pentaerythrite two phosphorusAcid esters; Wherein, the mol ratio of phosphoric acid and pentaerythrite is 1-3: 1;
Synthesizing of step 3, pentaerythritol diphosphate melamine-Lauxite salt:
In the melamine-Lauxite preparing to step 1, under stirring, dropwise add step 2The pentaerythritol diphosphate preparing, melamine-Lauxite used and pentaerythritol diphosphateMass ratio be 1-2: 1, after adding completely, at 60 DEG C, react 10-30min, make pentaerythrite two phosphorusAcid esters melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant.
Feature of the present invention is also, in described step 1, the mass fraction of formalin used is 37-42%.
Feature of the present invention is also, in described step 1, carries out synthetic anti-of melamine-LauxiteBetween seasonable, be 2.5h.
Feature of the present invention is also, in described step 1, regulating pH value with monoethanolamine is 8.5.
Beneficial effect of the present invention is as follows:
The present invention using preparation melamine-Lauxite as source of the gas, with preparation pentaerythrite diphosphonic acidEster carries out homogeneous reaction and prepares Amino Resinous Intumescent Flame Retardant, and the amino resins type preparing expands and hindersFire agent, can keep the excellent fire-retardancy of Caged bicyclic phosphate, can reduce costs again, to polymeric materialThe impact of material physical property is little, nonhygroscopic, and preparation process adopts water as solvent, meets environmental protection demand for development, toolThere is sizable application development prospect.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, below will be to implementingIn example or description of the Prior Art, the accompanying drawing of required use is briefly described, and apparently, the following describesIn accompanying drawing be only some embodiments of the present invention, for those of ordinary skill in the art, do not payingGo out under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 shows for preparation method's flow process of a kind of Amino Resinous Intumescent Flame Retardant that the embodiment of the present invention providesIntention;
Fig. 2 is that the present invention is the infrared spectrogram that the present invention prepares gained PDP;
Fig. 3 is the infrared spectrogram of the large molecule expanding fire retardant for preparing of the present invention;
Fig. 4 is the thermal multigraph of the large molecule expanding fire retardant prepared of the present invention.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and realityExecute example, the present invention is further elaborated. Only should be appreciated that specific embodiment described hereinOnly, in order to explain the present invention, be not intended to limit the present invention.
The system of a kind of Amino Resinous Intumescent Flame Retardant that the embodiment of the present invention that what Fig. 1 was exemplary show providesPreparation Method schematic flow sheet. As shown in Figure 1, a kind of amino resins type that the embodiment of the present invention provides expands and hindersThe preparation method of combustion agent, comprises the following steps:
Synthesizing of step S101, melamine-Lauxite:
Formalin is joined in container, and regulating pH value with monoethanolamine is 8-10, then according to mol ratio,Formaldehyde: urea: melamine=3-5: 0.2-1: 1, point 3 batches of mixtures by urea and melamine addIn formalin, stir, at 85-95 DEG C, react 1-3 hour, obtain thickness transparence trimerizationCyanamide-Lauxite;
Synthesizing of step S102, pentaerythritol diphosphate:
Taking phosphoric acid and pentaerythrite as initiation material, water, as solvent, stirs, and is warming up to100-140 DEG C is reacted, and the reaction time is 2-5h, separates water outlet, obtains thick pentaerythrite two phosphorusAcid esters; Wherein, the mol ratio of phosphoric acid and pentaerythrite is 1-3: 1;
Synthesizing of step S103, pentaerythritol diphosphate melamine-Lauxite salt:
In the melamine-Lauxite preparing to step S101, under stirring, dropwise add stepThe pentaerythritol diphosphate that S102 prepares, melamine-Lauxite used and pentaerythrite two phosphorusThe mass ratio of acid esters is 1-2: 1, after adding completely, at 60 DEG C, react 10-30min, and make pentaerythriteBisphosphate melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant
In embodiments of the present invention, in step S101, the mass fraction of formalin used is 37-42%.
In embodiments of the present invention, in step S101, carry out the synthetic reaction of melamine-LauxiteTime is 2.5h.
In embodiments of the present invention, in step S101, regulating pH value with monoethanolamine is 8.5.
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
A kind of Amino Resinous Intumescent Flame Retardant, obtains according to the method for being prepared as follows:
Step 1, the formalin that is 37% by mass fraction join thermometer, agitator, backflow are housedIn the there-necked flask of condenser pipe, regulating pH value with monoethanolamine is 8.5, utilizes temperature adjustment heating jacket to heat,According to mol ratio, formaldehyde: urea: melamine=3.5: 0.5: 1, points 3 batches by urea and melamineMixture joins in formalin, stirs, and reacts 2.5 hours at 90 DEG C, obtains thickness transparentShape melamine-Lauxite (being called for short MUF);
Step 2, according to the mol ratio of phosphoric acid and pentaerythrite 2: 1, take respectively pentaerythrite and 85%Phosphoric acid, with phosphoric acid and pentaerythrite initiation material, water, as solvent, joins agitator, thermometer is housedIn the four-hole bottle of reflux condenser, to stir, and be warming up to 120 DEG C and react, the reaction time is4h, separates water outlet, obtains thick pentaerythritol diphosphate (PDP);
In step 3, melamine-Lauxite of preparing to step 1, under stirring, dropwise addThe pentaerythritol diphosphate that step 2 prepares, melamine-Lauxite used and pentaerythrite twoThe mass ratio of phosphate is 1: 1, after adding completely, at 60 DEG C, reacts 20min, makes pentaerythrite twoPhosphate melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant.
Embodiment 2:
A kind of Amino Resinous Intumescent Flame Retardant, obtains according to the method for being prepared as follows:
Step 1, the formalin that is 40% by mass fraction join thermometer, agitator, backflow are housedIn the there-necked flask of condenser pipe, regulating pH value with monoethanolamine is 8, utilizes temperature adjustment heating jacket to heat,According to mol ratio, formaldehyde: urea: melamine=4.5: 0.2: 1, points 3 batches by urea and melamineMixture joins in formalin, stirs, and reacts 1 hour at 95 DEG C, obtains thickness transparenceMelamine-Lauxite (being called for short MUF);
Step 2, according to the mol ratio of phosphoric acid and pentaerythrite 1: 1, take respectively pentaerythrite and 85%Phosphoric acid, with phosphoric acid and pentaerythrite initiation material, water, as solvent, joins agitator, thermometer is housedIn the four-hole bottle of reflux condenser, to stir, and be warming up to 140 DEG C and react, the reaction time is2h, separates water outlet, obtains thick pentaerythritol diphosphate (PDP);
In step 3, melamine-Lauxite of preparing to step 1, under stirring, dropwise addThe pentaerythritol diphosphate that step 2 prepares, melamine-Lauxite used and pentaerythrite twoThe mass ratio of phosphate is 2: 1, after adding completely, at 60 DEG C, reacts 30min, makes pentaerythrite twoPhosphate melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant.
Embodiment 3:
A kind of Amino Resinous Intumescent Flame Retardant, obtains according to the method for being prepared as follows:
Step 1, the formalin that is 42% by mass fraction join thermometer, agitator, backflow are housedIn the there-necked flask of condenser pipe, regulating pH value with monoethanolamine is 9.5, utilizes temperature adjustment heating jacket to heat,According to mol ratio, formaldehyde: urea: melamine=3: 0.8: 1, points 3 batches by urea and melamineMixture joins in formalin, stirs, and reacts 3 hours at 85 DEG C, obtains thickness transparenceMelamine-Lauxite (being called for short MUF);
Step 2, according to the mol ratio of phosphoric acid and pentaerythrite 2.5: 1, take respectively pentaerythrite and 85%Phosphoric acid, with phosphoric acid and pentaerythrite initiation material, water, as solvent, joins agitator, thermometer is housedIn the four-hole bottle of reflux condenser, to stir, and be warming up to 100 DEG C and react, the reaction time is5h, separates water outlet, obtains thick pentaerythritol diphosphate (PDP);
In step 3, melamine-Lauxite of preparing to step 1, under stirring, dropwise addThe pentaerythritol diphosphate that step 2 prepares, melamine-Lauxite used and pentaerythrite twoThe mass ratio of phosphate is 1.5: 1, after adding completely, at 60 DEG C, reacts 10min, makes pentaerythriteBisphosphate melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant.
Embodiment 4:
A kind of Amino Resinous Intumescent Flame Retardant, obtains according to the method for being prepared as follows:
Step 1, the formalin that is 37% by mass fraction join thermometer, agitator, backflow are housedIn the there-necked flask of condenser pipe, regulating pH value with monoethanolamine is 10, utilizes temperature adjustment heating jacket to heat,According to mol ratio, formaldehyde: urea: melamine=5: 1: 1, point 3 batches of mixing urea and melamineCompound joins in formalin, stirs, and at 92 DEG C, reacts 80min, obtains thickness transparence threePoly cyanamid-Lauxite (being called for short MUF);
Step 2, according to the mol ratio of phosphoric acid and pentaerythrite 1.5: 1, take respectively pentaerythrite and 85%Phosphoric acid, with phosphoric acid and pentaerythrite initiation material, water, as solvent, joins agitator, thermometer is housedIn the four-hole bottle of reflux condenser, to stir, and be warming up to 120 DEG C and react, the reaction time is3.5h, separates water outlet, obtains thick pentaerythritol diphosphate (PDP);
In step 3, melamine-Lauxite of preparing to step 1, under stirring, dropwise addThe pentaerythritol diphosphate that step 2 prepares, melamine-Lauxite used and pentaerythrite twoThe mass ratio of phosphate is 1.2: 1, after adding completely, at 60 DEG C, reacts 25min, makes pentaerythriteBisphosphate melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant.
Adopt MAGNAIR-560 type infrared spectrometer to the pentaerythrite two of preparing in the embodiment of the present inventionPhosphate (PDP) carries out infrared spectrum analysis. Fig. 2 is the infrared light that the embodiment of the present invention is prepared gained PDPSpectrogram. As shown in Figure 2,3328cm-1Near be-OH stretching vibration absorption, 2938cm-1、2890cm-1Respectively CH2Antisymmetric stretching vibration and symmetrical stretching vibration absorb, 1207cm-1For the stretching vibration of P=OPeak. 1020,880,780 is spirane structure stretching vibration peak. Its infrared spectrogram has shown the dicyclo of PDPCage structure.
The amino resins type expandable flame retardant that adopts MAGNAIR-560 type infrared spectrometer to prepare the present inventionInfrared spectrum analysis is carried out in agent. Fig. 3 is the infrared of the Amino Resinous Intumescent Flame Retardant for preparing of the present inventionSpectrogram. As shown in Figure 3,3328cm-1Near be-OH and NH stretching vibration absorption, 2938cm-1、 2890cm-1Respectively CH2Antisymmetric stretching vibration and symmetrical stretching vibration absorb, 1521cm-1Near triazineThe C=N of ring absorbs and 814cm-1The characteristic absorption of place's triazine ring, 1016cm-1Place is first hydroxyl-CH2OH inhalesReceive 1240～1280cm-1For the stretching vibration peak of P=O. 1020,880,780,655cm-1For volution knotStructure stretching vibration peak. Above-mentioned each characteristic peak has characterized the basic structure of fire retardant, and the resistance that the present invention obtains is describedCombustion agent can be good at keeping the bicyclo cage shaped structure of PDP.
Amino Resinous Intumescent Flame Retardant prepared by the present invention carries out thermogravimetric analysis. Fig. 4 is prepared ammoniaThe thermal multigraph of base resin type expanding fire retardant. As shown in Figure 4, the pyrolysis initial decomposition temperature of fire retardant is182 DEG C, weight loss rate maximum 212 DEG C time, finally surplus charcoal 31.3%.
Amino Resinous Intumescent Flame Retardant prepared by the present invention carries out the mensuration of burst size of methanal, measurement resultAs shown in table 1. Table 1 has been listed the burst size of methanal in fire retardant of the present invention a week.
The burst size of methanal mg/L of table 1 fire retardant
As shown in Table 1, Amino Resinous Intumescent Flame Retardant prepared by the present invention, the burst size of formaldehyde is in timePass constantly and reduce, after the 5th day, the burst size of formaldehyde tends towards stability, but all lower than German El level markAccurate 10mg/100g.
Melmac has good anti-flammability and heat endurance, but due to the melmac degree of cross linkingCompared with high and easily solidify, therefore in prior art, the amino resins type that makes to utilize melmac to prepare is swollenIn swollen fire retardant, phosphorus content is compared with low and flame retardant effect is undesirable. Preparation method of the present invention does with amino resinsFor the source of the gas of expanding fire retardant, prepare amino resins type expansion resistance with pentaerythritol diphosphate homogeneous reactionCombustion agent. The present invention studies discovery, adds appropriate urea can improve amino resins type swollen at melmacThe phosphorus content of swollen fire retardant. Therefore adopt the modifier of urea as melamine resin, prepared onePlant modified melamine-formaldehyde resin, the i.e. prepared melamine-Lauxite of the first step of the present invention(MUF), then utilize prepared melamine-Lauxite (MUF) and the season penta preparingTetrol bisphosphate (PDP) reacts, and makes pentaerythritol diphosphate melamine-Lauxite salt,Be described Amino Resinous Intumescent Flame Retardant, make it to there is excellent fire resistance.
Obviously, those skilled in the art can carry out various changes and modification and not depart from this present inventionBright spirit and scope. Like this, if of the present invention these amendment and modification belong to the claims in the present invention andWithin the scope of its equivalent technologies, the present invention be also intended to comprise these change and modification interior.

Claims (4)

1. a preparation method for Amino Resinous Intumescent Flame Retardant, is characterized in that, comprises the steps:
Synthesizing of step 1, melamine-Lauxite:
Formalin is joined in container, and regulating pH value with monoethanolamine is 8-10, then according to mol ratio,Formaldehyde: urea: melamine=3-5: 0.2-1: 1, point 3 batches of mixtures by urea and melamine addIn formalin, stir, at 85-95 DEG C, react 1-3 hour, obtain thickness transparence trimerizationCyanamide-Lauxite;
Synthesizing of step 2, pentaerythritol diphosphate:
Taking phosphoric acid and pentaerythrite as initiation material, water, as solvent, stirs, and is warming up to100-140 DEG C is reacted, and the reaction time is 2-5h, separates water outlet, obtains thick pentaerythrite two phosphorusAcid esters; Wherein, the mol ratio of phosphoric acid and pentaerythrite is 1-3: 1;
Synthesizing of step 3, pentaerythritol diphosphate melamine-Lauxite salt:
In the melamine-Lauxite preparing to step 1, dropwise add step 2 to make at stirringThe standby pentaerythritol diphosphate obtaining, melamine-Lauxite used and pentaerythritol diphosphateMass ratio is 1-2: 1, after having added, at 60 DEG C, react 10-30min, and make pentaerythrite diphosphonic acidEster melamine-Lauxite salt, i.e. described Amino Resinous Intumescent Flame Retardant.
2. the method for claim 1, is characterized in that, in described step 1, formaldehyde used is moltenThe mass fraction of liquid is 37-42%.
3. the method for claim 1, is characterized in that, in described step 1, carries out melamineThe synthetic reaction time of amine-Lauxite is 2.5h.
4. the method for claim 1, is characterized in that, in described step 1, adjusts with monoethanolamineJoint pH value is 8.5.
CN201610077109.4A 2016-01-30 2016-01-30 Preparation method of amino resin type intumescent flame retardant Pending CN105601858A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107955845A (en) * 2017-11-01 2018-04-24 天津科技大学 A kind of preparation method of formaldehydeless intumescent leather combustion inhibitor special
CN108559047A (en) * 2018-01-27 2018-09-21 华北科技学院 A kind of preparation method of flame retardant polyurethane interpenetrating net polymer

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CN105131784A (en) * 2015-09-30 2015-12-09 华北科技学院 Intumescent fire-retardant coating and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN105131784A (en) * 2015-09-30 2015-12-09 华北科技学院 Intumescent fire-retardant coating and preparation method thereof

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MING GAO ET AL.: ""Thermal degradation and flame retardancy of rigid polyurethane foams containing a novel intumescent flame retardant"", 《J THERM ANAL CALORIM》 *
高明等: ""含季戊四醇二磷酸酯三聚氰胺-尿醛树脂盐环氧树脂的阻燃性能"", 《过程工程学报》 *
高明等: ""氨基树脂型膨胀阻燃剂的合成及应用研究"", 《北京理工大学学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107955845A (en) * 2017-11-01 2018-04-24 天津科技大学 A kind of preparation method of formaldehydeless intumescent leather combustion inhibitor special
CN107955845B (en) * 2017-11-01 2021-01-12 天津科技大学 Preparation method of special formaldehyde-free intumescent flame retardant for leather
CN108559047A (en) * 2018-01-27 2018-09-21 华北科技学院 A kind of preparation method of flame retardant polyurethane interpenetrating net polymer

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