CN105820518A - Preparation method for modified polyol with ultrahigh temperature resistance and high flame resistance - Google Patents
Preparation method for modified polyol with ultrahigh temperature resistance and high flame resistance Download PDFInfo
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- CN105820518A CN105820518A CN201510857050.6A CN201510857050A CN105820518A CN 105820518 A CN105820518 A CN 105820518A CN 201510857050 A CN201510857050 A CN 201510857050A CN 105820518 A CN105820518 A CN 105820518A
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Abstract
The invention provides a preparation method for modified polyol with ultrahigh temperature resistance and high flame resistance. The preparation method comprises the following steps: adding a mixture A produced by zirconate, phenol, phthalic anhydride, bisphenol A and pentaerythritol into a reaction vessel, then adding a catalyst, i.e., p-toluenesulfonic acid, into the reaction vessel and heating the reaction vessel to 150 to 200 DEG C for 6 to 8 h so as to produce a mixture phenol zirconate, i.e., a material B; subjecting the material B, liquid organosilicon and soluble glass to stirring at a temperature of 60 to 80 DEG C for 1 to 2 h so as to produce a material C; mixing the material C with solid formaldehyde to produce a material D, adding the material D into the reaction vessel, adding melamine into the reaction vessel so as to produce a material E, then adding polyethylene polyamine accounting for 15 to 70% of the total weight of the material D, heating the reaction vessel to 60 to 120 DEG C and carrying out a reaction for 6 to 10 h so as to produce a material F; mixing the material F with ultrafine expandable graphite and ultrafine APP under stirring so as to produce a material G; and heating the material G to 60 to 100 DEG C, adding polyphosphazene accounting for 0.1 to 6% of the total weight of the material G and then carrying out cooling to room temperature so as to produce the modified polyol with ultrahigh temperature resistance and high flame resistance.
Description
Technical field
The present invention relates to a kind of thermostable high fire-retardance modified polyalcohol preparation method, belong to modified polyalcohol preparation method technical field.
Background technology
The fire-protection rating of building organic insulation material is inadequate, it is easy to causing fire, once breaking out of fire, the people's lives and property will be by grave danger.CCTV's big fire then is finally assert, the finishing material fire-protection standard that BeiPeiLou curtain wall is chosen is less than the B level (being equivalent to the B1 level of GB/8624-2012) of national standard, but C level the most up to standard (being equivalent to the B2 level of GB/8624-2012).Curtain wall fire proofing material is the most up to standard, is to cause CCTV's big fire to occur and spread the most rapidly the key factor in full building, loses huge.Existing fire proofing grade is mostly below the B1 level of GB/8624-2012, and oxygen index (OI) is generally between 22～27%, and the grade improving fire proofing is the important topic that we study.
Summary of the invention
The invention aims to solve the problem that above-mentioned prior art exists, and then a kind of thermostable high fire-retardance modified polyalcohol preparation method is provided.
It is an object of the invention to be achieved through the following technical solutions:
A kind of thermostable high fire-retardance modified polyalcohol preparation method, step is as follows:
Step one, zirconic acid fat, phenol, phthalic anhydride, bisphenol-A and tetramethylolmethane are generated mixture A with the part by weight of 1 0.5～1.5 0.05～0.2 0.5～1.5 0.08～0.3 add in reactor, reactor adds catalyst Dibutyltin oxide, catalyst Dibutyltin oxide accounts for the 1～5 ‰ of mixture A gross weight, reactor is heated to 150～240 DEG C, generates phenol zirconic acid fat i.e. material B after 6～8 hours.
Step 2, material B, liquid silicone and waterglass stir at a temperature of 60～80 DEG C 1～2 hour with the part by weight of 1 0.01～0.1 0.01～0.3 and generate material C.
Step 3, material C and solid formaldehyde mix generation material D with the part by weight of 1～3 0.5～2 and add in reactor, reactor adds the tripolycyanamide generation material E accounting for material D gross weight 15～40, adding the polyethylene polyamine accounting for material D gross weight 15～70, reactor is heated up to 60～150 DEG C of reactions and generates material F in 6～10 hours.
Step 4, material F and ultra-fine expansible graphite, ultra-fine APP stir mixing with the part by weight of 0.5～2.5 0.08～0.35 0.5～1.5 and generate material G.
Step 5, material G is warming up to 60～100 DEG C of 0.1～polyphosphazenes of 6% adding material G gross weights, is down to after room temperature generate thermostable high fire-retardance modified polyalcohol.
The characteristic synergism that each raw material of the present invention is different, is allowed to organically combine thus reaches optimum resistance combustion effect, and fire-protection rating can reach B1 to the A2 level of GB/8624-2012.
Thermostable high fire-retardance modified polyalcohol prepared by the present invention is mainly for the production of polyurethane flexible flame-retardant foam and rigid poly urethanes flame-retardant foam, the Sandwich board such as built, building heat preservation spraying etc., it is particularly suited for high flame retardant hard polyurethane foam, such that it is able to be substantially reduced the consumption of fire retardant.For synthesizing flame-retardant hard polyurethane foam, there is higher anti-flammability, oxygen index (OI) >=35% (oxygen index method GB2406-80).Occasion at building, insulation and some special flame-proof polyols is with a wide range of applications.
Detailed description of the invention
The present invention is described in further detail below: the present embodiment is implemented under premised on technical solution of the present invention, gives detailed embodiment, but protection scope of the present invention is not limited to following embodiment.
A kind of thermostable high fire-retardance modified polyalcohol preparation method involved by the present embodiment, step is as follows:
Step one, zirconic acid fat, phenol, phthalic anhydride, bisphenol-A and tetramethylolmethane are generated mixture A with the part by weight of 1 0.5～1.5 0.05～0.2 0.5～1.5 0.08～0.3 add in reactor, reactor adds catalyst Dibutyltin oxide, catalyst Dibutyltin oxide accounts for the 1～5 ‰ of mixture A gross weight, reactor is heated to 150～240 DEG C, generates phenol zirconic acid fat i.e. material B after 6～8 hours.
Step 2, material B, liquid silicone and waterglass stir at a temperature of 60～80 DEG C 1～2 hour with the part by weight of 1 0.01～0.1 0.01～0.3 and generate material C.
Step 3, material C and solid formaldehyde mix generation material D with the part by weight of 1～3 0.5～2 and add in reactor, reactor adds the tripolycyanamide generation material E accounting for material D gross weight 15～40, adding the polyethylene polyamine accounting for material D gross weight 15～70, reactor is heated up to 60～150 DEG C of reactions and generates material F in 6～10 hours.
Step 4, material F and ultra-fine expansible graphite, ultra-fine APP stir mixing with the part by weight of 0.5～2.5 0.08～0.35 0.5～1.5 and generate material G.
Step 5, material G is warming up to 60～100 DEG C of 0.1～polyphosphazenes of 6% adding material G gross weights, is down to after room temperature generate thermostable high fire-retardance modified polyalcohol.
In described step one, the optimum weight ratio of zirconic acid fat, phenol, phthalic anhydride, bisphenol-A and tetramethylolmethane is 11 0.1 1 0.1.
In described step 2, the optimum weight ratio of material B, liquid silicone and waterglass is 1 0.05 0.15.
In described step 3, the optimum weight ratio of material C and solid formaldehyde is 21.
In described step 4, the optimum weight ratio of material F and ultra-fine expansible graphite, ultra-fine APP is 1.5 0.2 1.
In described step 5, the polyphosphazene of the 3% of addition material G gross weight.
The above; it is only the present invention preferably detailed description of the invention; these detailed description of the invention are all based on the different implementations under general idea of the present invention; and protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope that the invention discloses; the change that can readily occur in or replacement, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. a thermostable high fire-retardance modified polyalcohol preparation method, it is characterised in that
Step one, zirconic acid fat, phenol, phthalic anhydride, bisphenol-A and tetramethylolmethane are generated mixture A with the part by weight of 1 0.5～1.5 0.05～0.2 0.5～1.5 0.08～0.3 add in reactor, reactor adds catalyst Dibutyltin oxide, catalyst Dibutyltin oxide accounts for the 1～5 ‰ of mixture A gross weight, reactor is heated to 150～240 DEG C, generates mixing phenol zirconic acid fat i.e. material B after 6～8 hours；
Step 2, material B, liquid silicone and waterglass stir at a temperature of 60～80 DEG C 1～2 hour with the part by weight of 1 0.01～0.1 0.01～0.3 and generate material C；
Step 3, material C and solid formaldehyde mix generation material D with the part by weight of 1～3 0.5～2 and add in reactor, reactor adds the tripolycyanamide generation material E accounting for material D gross weight 15～40, adding the polyethylene polyamine accounting for material D gross weight 15～70, reactor is heated up to 60～150 DEG C of reactions and generates material F in 6～10 hours；
Step 4, material F and ultra-fine expansible graphite, ultra-fine APP stir mixing with the part by weight of 0.5～2.5 0.08～0.35 0.5～1.5 and generate material G；
Step 5, material G is warming up to 60～100 DEG C of 0.1～polyphosphazenes of 6% adding material G gross weights, is down to after room temperature generate thermostable high fire-retardance modified polyalcohol.
Thermostable high fire-retardance modified polyalcohol preparation method the most according to claim 1, it is characterised in that in described step one, the part by weight of zirconic acid fat, phenol, phthalic anhydride, bisphenol-A and tetramethylolmethane is 11 0.1 1 0.1.
Thermostable high fire-retardance modified polyalcohol preparation method the most according to claim 1, it is characterised in that in described step 2, the part by weight of material B, liquid silicone and waterglass is 1 0.05 0.15.
Thermostable high fire-retardance modified polyalcohol preparation method the most according to claim 1, it is characterised in that in described step 3, the part by weight of material C and solid formaldehyde is 21, and material D and many polycaprolactam polyamines weight ratio are 21.
Thermostable high fire-retardance modified polyalcohol preparation method the most according to claim 1, it is characterised in that in described step 4, the part by weight of material F and ultra-fine expansible graphite, ultra-fine APP is 1.5 0.2 1.
Thermostable high fire-retardance modified polyalcohol preparation method the most according to claim 1, it is characterised in that in described step 5, the polyphosphazene of the 3% of addition material G gross weight.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106220809A (en) * | 2016-08-05 | 2016-12-14 | 潍坊远航聚氨酯保温材料有限公司 | A kind of high fire-retardance graphite coating polyurethane and preparation method thereof and construction method |
| CN107236092A (en) * | 2017-07-20 | 2017-10-10 | 中海石油(中国)有限公司 | One kind contains silicate sturcture monomer and preparation method and application |
| CN113512227A (en) * | 2021-04-13 | 2021-10-19 | 何顺伦 | High-flame-retardant PET (polyethylene terephthalate) foam material and preparation method thereof |
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| CN102027033A (en) * | 2008-05-20 | 2011-04-20 | 旭硝子株式会社 | Manufacturing method for hard polyurethane foam |
| CN104861144A (en) * | 2015-04-28 | 2015-08-26 | 南通苏东新型外墙保温板有限公司 | Flame retardant hard bubble polyurethane |
| CN104877102A (en) * | 2015-06-03 | 2015-09-02 | 威海云山科技有限公司 | Flame-retardant rigid polyurethane foam heat insulation plate |
| CN105085853A (en) * | 2015-02-27 | 2015-11-25 | 大连亚泰科技新材料股份有限公司 | Preparation method of halogen-free flame retardant rigid polyurethane foam insulation material for exterior wall insulation |
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Patent Citations (4)
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| CN102027033A (en) * | 2008-05-20 | 2011-04-20 | 旭硝子株式会社 | Manufacturing method for hard polyurethane foam |
| CN105085853A (en) * | 2015-02-27 | 2015-11-25 | 大连亚泰科技新材料股份有限公司 | Preparation method of halogen-free flame retardant rigid polyurethane foam insulation material for exterior wall insulation |
| CN104861144A (en) * | 2015-04-28 | 2015-08-26 | 南通苏东新型外墙保温板有限公司 | Flame retardant hard bubble polyurethane |
| CN104877102A (en) * | 2015-06-03 | 2015-09-02 | 威海云山科技有限公司 | Flame-retardant rigid polyurethane foam heat insulation plate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220809A (en) * | 2016-08-05 | 2016-12-14 | 潍坊远航聚氨酯保温材料有限公司 | A kind of high fire-retardance graphite coating polyurethane and preparation method thereof and construction method |
| CN107236092A (en) * | 2017-07-20 | 2017-10-10 | 中海石油(中国)有限公司 | One kind contains silicate sturcture monomer and preparation method and application |
| CN107236092B (en) * | 2017-07-20 | 2019-07-16 | 中海石油(中国)有限公司 | One kind containing silicate sturcture monomer and the preparation method and application thereof |
| CN113512227A (en) * | 2021-04-13 | 2021-10-19 | 何顺伦 | High-flame-retardant PET (polyethylene terephthalate) foam material and preparation method thereof |
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