CN104262607A - Flame-retardant polyether polyol using melamine as basic feature structure and preparation method thereof - Google Patents
Flame-retardant polyether polyol using melamine as basic feature structure and preparation method thereof Download PDFInfo
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- CN104262607A CN104262607A CN201410454234.3A CN201410454234A CN104262607A CN 104262607 A CN104262607 A CN 104262607A CN 201410454234 A CN201410454234 A CN 201410454234A CN 104262607 A CN104262607 A CN 104262607A
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Abstract
The invention discloses flame-retardant polyether polyol using melamine as a basic feature structure and a preparation method thereof. The flame-retardant polyether polyol using melamine as the basic feature structure is prepared from the following components in parts by weight: 5-20 parts of melamine, 5-30 parts of formaldehyde, 0.01-0.1 part of an alkali regulator, 2-10 parts of a co-initiator, 50-100 parts of epoxy chloropropane and 0.01-2.0 parts of a catalyst. The preparation method comprises the following steps: mixing melamine, formaldehyde and the alkali regulator, and heating to 65-75 DEG C to react for 35-45 minutes; and adding the co-initiator, the catalyst and epoxy chloropropane into the prepared reaction liquid, heating to 70-100 DEG C to react for 10-24 hours, and distilling at 100-130 DEG C and -0.1MPa to obtain the flame-retardant polyether polyol using melamine as the basic feature structure. The preparation method has the characteristics of mild reacting condition, easily implemented operation, low production cost and the like.
Description
Technical field
The present invention relates to a kind of is flame retardant polyether polyol levying structure and preparation method thereof substantially with trimeric cyanamide, belongs to Polymer Synthesizing research field.
Background technology
Conventional polyether polyols refers to what active hydrogen compounds obtained in certain temperature and pressure ring-opening polymerization with epoxy compounds (comprising propylene oxide, oxyethane etc.) in the presence of a catalyst.Such polyether glycol is for the production of urethane foam.But the porous plastics oxygen index prepared of polyether glycol is generally below 19 thus, belongs to inflammable material.
At present, mainly contain two kinds to the processing mode of polyether glycol flame retardant properties, one is the mode of adding fire retardant; Two is give polyether glycol segment flame retarding construction or ignition-proof element to reach fire-retardant object, i.e. reactive flame retardant; But there is easily migration, flame retardant effect can not be kept lastingly and destroy the shortcomings such as foam physics performance in additive flame retardant, slowly can not meet the demand that people are growing to hard polyurethane foam, and reactive flame retardant can avoid a series of defects of additive flame retardant.
Existing reaction-type flame-retarding polyether glycol mainly contains phosphorus system, Halogen, phosphorus halogen system, nitrogen system, compound flame retardant polyether polyol, wherein phosphorus halogen system uses the most extensive, can Halogen, to there is synthesis material price in nitrogenous flame retardant polyether polyol high, porous plastics prepared therefrom problems such as smog is large when burning, toxicity is high and be limited to use.
Nitrogen system flame retardant polyether polyol relative environmental protection, it meets current highly effective flame-retardant, burning discharges the trend that smog is low, toxicity is little.But there is the relatively high technical problem of process relative complex, cost in its preparation method.
Summary of the invention
One of the object of the invention is poor in order to solve above-mentioned conventional polyether polyols flame retardant properties; Add fire retardant type polyether glycol to there is easily migration, flame retardant effect can not be kept lastingly; It is the flame retardant polyether polyol substantially levying structure compared with high-technology problem with trimeric cyanamide that reaction-type flame-retarding polyether glycol synthetic method relative complex, cost provide a kind of, should be that the flame retardant polyether polyol substantially levying structure has intrinsic flame-retarding characteristic with trimeric cyanamide, production cost be also lower.
Two of object of the present invention be to provide above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, it is simple that the method has preparation process, the advantage such as can to complete at ambient pressure.
technical scheme of the present invention
Be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, calculate by weight, its raw material composition and content as follows:
Trimeric cyanamide 5 ~ 20 parts
15 ~ 30 parts, formaldehyde
Alkaline conditioner 0.01 ~ 0.1 part
Initiator 2 ~ 10 parts altogether
Epoxy chloropropane 50 ~ 100 parts
Catalyzer 0.01 ~ 2.0 part
Wherein said formaldehyde to be mass percent concentration be 35 ~ 40% formalin;
Described alkaline conditioner to be mass percent concentration be 10 ~ 50% the NaOH aqueous solution, the mass percent concentration KOH aqueous solution that is 10 ~ 50%, the mass percent concentration sodium bicarbonate aqueous solution that is 5 ~ 10%, mass percent concentration be 5 ~ 10% triethylamine aqueous solution, mass percent concentration be 5 ~ 10% diethylamine aqueous solution or mass percent concentration be the ammonia soln of 5 ~ 25%;
Described common initiator is ethylene glycol, glycerol, BDO, trolamine, diethanolamine, sucrose or TriMethylolPropane(TMP), is preferably glycerol, BDO, trolamine or sucrose;
Described catalyzer to be mass percent concentration be 10 ~ 50% the NaOH aqueous solution, mass percent concentration be 10 ~ 50% the KOH aqueous solution, boron trifluoride ethyl ether complex or bimetallic catalyst, be preferably mass percent concentration be 10 ~ 50% the NaOH aqueous solution, mass percent concentration be 10 ~ 50% the KOH aqueous solution or boron trifluoride ethyl ether complex.
Above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, namely carry out being obtained by reacting many melamine methylols under the condition of alkalescence with trimeric cyanamide and formaldehyde, it is the flame retardant polyether polyol substantially levying structure that many melamine methylols of gained synthesize with trimeric cyanamide with epoxy chloropropane under the existence of common initiator, catalyzer, and concrete steps are as follows:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 65 ~ 75 DEG C and carry out reaction 35 ~ 45min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of many melamine methylols of step (1) gained, stir and be heated to 70 ~ 100 DEG C and carry out reaction 10 ~ 24 h, then it is 100 ~ 130 DEG C by the reaction solution control temperature of gained, be preferably 120 DEG C, pressure is-0.1MPa, 1 ~ 2 h is to steam the small molecules such as solvent in distillation, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
Above-mentioned preparation method's gained be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, through NEXUS870 type fourier transform infrared spectrometry (Nicolet company of the U.S.) scanning, at 1610 ~ 1616 cm
-1, 1520 cm
-1, 814 cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide; Adopt Tetra hydro Phthalic anhydride pyridine method to measure, its hydroxyl value is 160.8 ~ 209.3mgKOH/g; Adopt NDJ-8S automatic digital display viscosity apparatus (Jia, Shenzhen City Kodak Electronic Science and Technology Co., Ltd.) to measure, its viscosity is 4583 ~ 12104mPa.s/25 DEG C; According to GB/T 12008.6, method measures, and its moisture is≤0.13%.
Beneficial effect of the present invention
Of the present invention is substantially in flame retardant polyether polyol levying structure and preparation method thereof with trimeric cyanamide, because trimeric cyanamide used has a stable carbon, nitrogen virtue heterocycle structure and three amino, nitrogen content is 66.7%, distil in thermal histories, volatilize, the thermo-negative reaction such as decomposition, discharge non-flammable gases, formed to expand on combustiblematerials surface and intercept carbon-coating, thus play fire retardation.By itself and formaldehyde reaction are obtained many melamine methylols, and then common initiator, catalyzer exist under with epoxy chloropropane ring-opening polymerization, be introduced into also Absorbable organic halogens existence in pfpe molecule segment in the mode of covalent linkage, make it have intrinsic flame-retarding characteristic.Polyether glycol preferably flame retardant properties can be given thus, solve the problem of conventional polyether polyols flame retardant properties difference.
Further, of the present invention is in the preparation method of the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, because synthesis material used is epoxy chloropropane, this raw material is cheap and easy to get, compared with conventional polyether polyols preparation method, without the need to carrying out in autoclave, and reaction conditions is gentle, processing ease is implemented, cheap.
Further, of the present invention take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, the hydroxyl value of gained trimeric cyanamide intrinsic structure flame retardant polyether polyol is 160.8 ~ 209.3 mgKOH/g, and viscosity is 4583 ~ 12104 mPa.s/25 DEG C, moisture≤0.13%.
Accompanying drawing explanation
Fig. 1, embodiment 1 gained take trimeric cyanamide as the infrared spectrogram of the flame retardant polyether polyol substantially levying structure.
Embodiment
Also by reference to the accompanying drawings the present invention is described in further detail below by embodiment, but do not limit the present invention.
The present invention's trimeric cyanamide used, formalin, alkaline conditioner, altogether initiator, epoxy chloropropane are all purchased from Shanghai traditional Chinese medicines group;
The catalyzer that the present invention is used, by Huaian, Ahmedabad urethane Science and Technology Ltd. provides.
embodiment 1
Be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, calculate by weight, its raw material composition and content as follows:
Trimeric cyanamide 7.5 parts
15 parts, formaldehyde
Alkaline conditioner 0.05 part
Initiator 3 parts altogether
Epoxy chloropropane 73 parts
Catalyzer 1.5 parts
Wherein said formaldehyde to be mass percent concentration be 37% formalin;
Described alkaline conditioner to be mass percent concentration be 30% the NaOH aqueous solution;
Described common initiator is glycerol;
Described catalyzer to be mass percent concentration be 30% the NaOH aqueous solution.
Above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, specifically comprise the following steps:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 70 DEG C and carry out reaction 37min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of many melamine methylols of step (1) gained, stir and be heated to 90 DEG C and carry out reaction 24 h, then by the reaction solution control temperature 120 DEG C of gained, pressure carries out distillation 1.5 h for-0.1MPa, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
Above-mentioned gained be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, through NEXUS870 type fourier transform infrared spectrometry (Nicolet company of the U.S.) scanning, its infrared spectrogram as shown in Figure 1, as can be seen from Figure 1, at 1613 cm
-1, 1520 cm
-1, 814 cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide, shows thus, and above-mentioned obtained flame-retardant polyether glycol is for substantially to levy structure with trimeric cyanamide.
Adopting Tetra hydro Phthalic anhydride pyridine method to measure its hydroxyl value is 206.7 mgKOH/g;
Adopting NDJ-8S automatic digital display viscosity apparatus to measure its viscosity is 4583 mPa.s/25 DEG C;
According to GB/T 12008.6, method measures its moisture is 0.13%.
embodiment 2
Be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, calculate by weight, its raw material composition and content as follows:
Trimeric cyanamide 6.5 parts
16.5 parts, formaldehyde
Alkaline conditioner 0.04 part
Initiator 3.3 parts altogether
Epoxy chloropropane 72 parts
Catalyzer 1.3 parts
Wherein said formaldehyde to be mass percent concentration be 35% formalin;
Described alkaline conditioner to be mass percent concentration be 20% the KOH aqueous solution;
Described common initiator is trolamine;
Described catalyzer to be mass percent concentration be 20% the KOH aqueous solution.
Above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, specifically comprise the following steps:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 75 DEG C and carry out reaction 35 min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of many melamine methylols of step (1) gained, stir and be heated to 85 DEG C and carry out reaction 22 h, then by the reaction solution control temperature 120 DEG C of gained, pressure carries out distillation 1 h for-0.1MPa, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
Above-mentioned be able to trimeric cyanamide is the flame retardant polyether polyol substantially levying structure, at 1615 cm
-1, 1522 cm
-1, 814 cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide; Its hydroxyl value is 163.9 mgKOH/g, viscosity is 9545 mPa.s/25 DEG C, moisture is 0.1%.
embodiment 3
Be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, calculate by weight, its raw material composition and content as follows:
Trimeric cyanamide 6.0 parts
20.5 parts, formaldehyde
Alkaline conditioner 0.05 part
Initiator 3.2 parts altogether
Epoxy chloropropane 70 parts
Catalyzer 0.5 part
Wherein said formaldehyde mass percent concentration is the formalin of 40%;
Described alkaline conditioner to be mass percent concentration be 10% triethylamine aqueous solution;
Described common initiator is trolamine;
Described catalyzer is boron trifluoride ethyl ether complex.
Above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, specifically comprise the following steps:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 65 DEG C and carry out reaction 45 min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of melamine methylol of step (1) gained, stir and be heated to 75 DEG C and carry out reaction 10 h, then by the reaction solution control temperature 120 DEG C of gained, pressure carries out distillation 1.5 h for-0.1MPa, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
Above-mentioned be able to trimeric cyanamide is the flame retardant polyether polyol substantially levying structure, at 1616cm
-1, 1523cm
-1, 814cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide; Its hydroxyl value is 160.8mgKOH/g, viscosity is 12104 mPa.s/25 DEG C, moisture is 0.06%.
embodiment 4
Be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, calculate by weight, it is former
Material composition and content as follows:
Trimeric cyanamide 5.0 parts
18.5 parts, formaldehyde
Alkaline conditioner 0.08 part
Initiator 3.5 parts altogether
Epoxy chloropropane 71.5 parts
Catalyzer 1.0 parts
Wherein said formaldehyde mass percent concentration is the formalin of 36%;
Described alkaline conditioner to be mass percent concentration be 5% diethylamine aqueous solution;
Described common initiator is BDO;
Described catalyzer to be mass percent concentration be 30% the NaOH aqueous solution.
Above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, specifically comprise the following steps:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 75 DEG C and carry out reaction 40 min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of many melamine methylols of step (1) gained, stir and be heated to 95 DEG C and carry out reaction 24 h, then by the reaction solution control temperature 120 DEG C of gained, pressure carries out distillation 1.5 h for-0.1MPa, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
Above-mentioned be able to trimeric cyanamide is the flame retardant polyether polyol substantially levying structure, at 1616cm
-1, 1525cm
-1, 814cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide; Its hydroxyl value is 170.6mgKOH/g, viscosity is 5833mPa.s/25 DEG C, moisture is 0.12%.
embodiment 5
Be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, calculate by weight, its raw material composition and content as follows:
Trimeric cyanamide 10.5 parts
22.5 parts, formaldehyde
Alkaline conditioner 0.04 part
Initiator 4.0 parts altogether
Epoxy chloropropane 63.5 parts
Catalyzer 0.02 part
Wherein said formaldehyde mass percent concentration is the formalin of 37%;
Described alkaline conditioner to be mass percent concentration be 5% sodium bicarbonate aqueous solution;
Described common initiator is sucrose;
Described catalyzer to be mass percent concentration be 20% the KOH aqueous solution.
Above-mentioned a kind of take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, specifically comprise the following steps:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 70 DEG C and carry out reaction 46 min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of many melamine methylols of step (1) gained, stir and be heated to 90 DEG C and carry out reaction 22 h, then by the reaction solution control temperature 120 DEG C of gained, pressure carries out distillation 2 h for-0.1MPa, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
Above-mentioned be able to trimeric cyanamide is the flame retardant polyether polyol substantially levying structure, at 1613 cm
-1, 1520 cm
-1, 814 cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide; Its hydroxyl value is 209.3 mgKOH/g, viscosity is 10994 mPa.s/25 DEG C, moisture is 0.08%.
In sum, of the present invention take trimeric cyanamide as the flame retardant polyether polyol substantially levying structure, because trimeric cyanamide is introduced on pfpe molecule main chain by covalent linkage, its carbon, nitrogen virtue heterocycle structure has good thermostability, can give the flame retardant properties that polyether glycol is better.The method is simple to operate, with low cost without the need to reaction under high pressure.Thus obtained with trimeric cyanamide be substantially levy structure flame retardant polyether polyol at 1610 ~ 1616 cm
-1, 1520 cm
-1, 814 cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide, and its hydroxyl value is 160.8 ~ 209.3 mgKOH/g, and viscosity is 4583 ~ 12104 mPa.s/25 DEG C, moisture≤0.13%.
Above said content be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (8)
1. be the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, it is characterized in that described is the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, at 1610 ~ 1616 cm
-1, 1520 cm
-1, 814 cm
-1wave number place all has the infrared signature absorption peak of trimeric cyanamide, and its hydroxyl value is 160.8 ~ 209.3 mgKOH/g, and viscosity is 4583 ~ 12104 mPa.s/25 DEG C, moisture≤0.13%;
Calculate by weight, described is that the raw material composition of the flame retardant polyether polyol substantially levying structure and content are as follows with trimeric cyanamide:
Trimeric cyanamide 5 ~ 20 parts
15 ~ 30 parts, formaldehyde
Alkaline conditioner 0.01 ~ 0.1 part
Initiator 2 ~ 10 parts altogether
Epoxy chloropropane 50 ~ 100 parts
Catalyzer 0.01 ~ 2.0 part
Wherein said formaldehyde to be mass percent concentration be 35 ~ 40% formalin;
Described alkaline conditioner to be mass percent concentration be 10 ~ 50% the NaOH aqueous solution, the mass percent concentration KOH aqueous solution that is 10 ~ 50%, the mass percent concentration sodium bicarbonate aqueous solution that is 5 ~ 10%, mass percent concentration be 5 ~ 10% triethylamine aqueous solution, mass percent concentration be 5 ~ 10% diethylamine aqueous solution or mass percent concentration be the ammonia soln of 5 ~ 25%;
Described common initiator is ethylene glycol, glycerol, BDO, trolamine, diethanolamine, sucrose or TriMethylolPropane(TMP);
Described catalyzer to be mass percent concentration be 10 ~ 50% the NaOH aqueous solution, mass percent concentration be 10 ~ 50% the KOH aqueous solution, boron trifluoride ethyl ether complex or bimetallic catalyst.
2. a kind of is as claimed in claim 1 the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, it is characterized in that calculating by weight, its raw material composition and content as follows:
Trimeric cyanamide 5 ~ 10.5 parts
15 ~ 22.5 parts, formaldehyde
Alkaline conditioner 0.04 ~ 0.08 part
Initiator 3 ~ 4.0 parts altogether
Epoxy chloropropane 63.5 ~ 73 parts
Catalyzer 0.02 ~ 1.5 part.
3. a kind of is as claimed in claim 2 the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, it is characterized in that calculating by weight, its raw material composition and content as follows:
Trimeric cyanamide 7.5 parts
15 parts, formaldehyde
Alkaline conditioner 0.05 part
Initiator 3 parts altogether
Epoxy chloropropane 73 parts
Catalyzer 1.5 parts
Wherein said formaldehyde to be mass percent concentration be 37% formalin;
Described alkaline conditioner to be mass percent concentration be 30% the NaOH aqueous solution;
Described common initiator is glycerol;
Described catalyzer to be mass percent concentration be 30% the NaOH aqueous solution.
4. a kind of is as claimed in claim 2 the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, it is characterized in that calculating by weight, its raw material composition and content as follows:
Trimeric cyanamide 6.5 parts
16.5 parts, formaldehyde
Alkaline conditioner 0.04 part
Initiator 3.3 parts altogether
Epoxy chloropropane 72 parts
Catalyzer 1.3 parts
Wherein said formaldehyde to be mass percent concentration be 35% formalin;
Described alkaline conditioner to be mass percent concentration be 20% the KOH aqueous solution;
Described common initiator is trolamine;
Described catalyzer to be mass percent concentration be 20% the KOH aqueous solution.
5. a kind of is as claimed in claim 2 the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, it is characterized in that, calculates by weight, its raw material composition and content as follows:
Trimeric cyanamide 6.0 parts
20.5 parts, formaldehyde
Alkaline conditioner 0.05 part
Initiator 3.2 parts altogether
Epoxy chloropropane 70 parts
Catalyzer 0.5 part
Wherein said formaldehyde mass percent concentration is the formalin of 40%;
Described alkaline conditioner to be mass percent concentration be 10% triethylamine aqueous solution;
Described common initiator is trolamine;
Described catalyzer is boron trifluoride ethyl ether complex.
6. a kind of is as claimed in claim 2 the flame retardant polyether polyol substantially levying structure with trimeric cyanamide, it is characterized in that calculating by weight, its raw material composition and content as follows:
Trimeric cyanamide 5.0 parts
18.5 parts, formaldehyde
Alkaline conditioner 0.08 part
Initiator 3.5 parts altogether
Epoxy chloropropane 71.5 parts
Catalyzer 1.0 parts
Wherein said formaldehyde mass percent concentration is the formalin of 36%;
Described alkaline conditioner to be mass percent concentration be 5% diethylamine aqueous solution;
Described common initiator is BDO;
Described catalyzer to be mass percent concentration be 30% the NaOH aqueous solution.
7. a kind of as claimed in claim 2 take trimeric cyanamide as the flame retardant polyether polyol substantially levying structure, its
Be characterised in that and calculate by weight, its raw material composition and content as follows:
Trimeric cyanamide 10.5 parts
22.5 parts, formaldehyde
Alkaline conditioner 0.04 part
Initiator 4.0 parts altogether
Epoxy chloropropane 63.5 parts
Catalyzer 0.02 part
Wherein said formaldehyde mass percent concentration is the formalin of 37%;
Described alkaline conditioner to be mass percent concentration be 5% sodium bicarbonate aqueous solution;
Described common initiator is sucrose;
Described catalyzer to be mass percent concentration be 20% the KOH aqueous solution.
8. a kind of as described in as arbitrary in claim 1 ~ 7 take trimeric cyanamide as the preparation method of the flame retardant polyether polyol substantially levying structure, it is characterized in that specifically comprising the steps:
(1), by trimeric cyanamide, formaldehyde mixing, add alkaline conditioner, then stir and be heated to 50 ~ 90 DEG C and carry out reaction 20 ~ 60min, obtain the reaction solution containing many melamine methylols;
(2), common initiator, catalyzer and epoxy chloropropane is added to containing in the reaction solution of many melamine methylols of step (1) gained, stir and be heated to 70 ~ 100 DEG C and carry out reaction 10 ~ 24 h, then by gained reaction solution control temperature 100 ~ 130 DEG C, pressure carries out distillation 1 ~ 2 h for-0.1MPa, and it is the flame retardant polyether polyol substantially levying structure that the residue after distillation is with trimeric cyanamide.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111777734A (en) * | 2020-08-07 | 2020-10-16 | 宁波耀众模塑科技有限公司 | Flame-retardant polyether material for polyurethane foaming product |
CN112300383A (en) * | 2020-10-21 | 2021-02-02 | 福建省天骄化学材料有限公司 | Flame-retardant polyether polyol and preparation method thereof |
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4939182A (en) * | 1988-07-27 | 1990-07-03 | The Dow Chemical Company | Melamine-alkanolamine condensates and polyurethanes prepared therefrom |
CN102432859A (en) * | 2011-08-24 | 2012-05-02 | 山东蓝星东大化工有限责任公司 | Synthesis method of flexible-foam flame-retardant polyether polyol |
CN103539932A (en) * | 2013-09-11 | 2014-01-29 | 江苏雅克科技股份有限公司 | Preparation method and applications of reaction type Mannich polyether polyol with permanent flame retardant effect |
CN103709395A (en) * | 2013-12-16 | 2014-04-09 | 中国林业科学研究院林产化学工业研究所 | Biomass base structure flame retardant polyol and preparation method and application thereof |
CN103897127A (en) * | 2014-04-21 | 2014-07-02 | 苏州科技学院相城研究院 | Flame-retardant polymeric MB compound and preparation method thereof |
-
2014
- 2014-09-09 CN CN201410454234.3A patent/CN104262607A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4939182A (en) * | 1988-07-27 | 1990-07-03 | The Dow Chemical Company | Melamine-alkanolamine condensates and polyurethanes prepared therefrom |
CN102432859A (en) * | 2011-08-24 | 2012-05-02 | 山东蓝星东大化工有限责任公司 | Synthesis method of flexible-foam flame-retardant polyether polyol |
CN103539932A (en) * | 2013-09-11 | 2014-01-29 | 江苏雅克科技股份有限公司 | Preparation method and applications of reaction type Mannich polyether polyol with permanent flame retardant effect |
CN103709395A (en) * | 2013-12-16 | 2014-04-09 | 中国林业科学研究院林产化学工业研究所 | Biomass base structure flame retardant polyol and preparation method and application thereof |
CN103897127A (en) * | 2014-04-21 | 2014-07-02 | 苏州科技学院相城研究院 | Flame-retardant polymeric MB compound and preparation method thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111777734A (en) * | 2020-08-07 | 2020-10-16 | 宁波耀众模塑科技有限公司 | Flame-retardant polyether material for polyurethane foaming product |
CN112300383A (en) * | 2020-10-21 | 2021-02-02 | 福建省天骄化学材料有限公司 | Flame-retardant polyether polyol and preparation method thereof |
CN112679722A (en) * | 2020-12-28 | 2021-04-20 | 山东一诺威新材料有限公司 | Preparation method of polyether polyol for all-water flame-retardant system |
CN112679722B (en) * | 2020-12-28 | 2023-03-07 | 山东一诺威新材料有限公司 | Preparation method of polyether polyol for all-water flame-retardant system |
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