CN104893641A - Preparation method of high-strength flame-retardant polyurethane sealant - Google Patents
Preparation method of high-strength flame-retardant polyurethane sealant Download PDFInfo
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- CN104893641A CN104893641A CN201510287516.3A CN201510287516A CN104893641A CN 104893641 A CN104893641 A CN 104893641A CN 201510287516 A CN201510287516 A CN 201510287516A CN 104893641 A CN104893641 A CN 104893641A
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Abstract
The invention discloses a preparation method of a high-strength flame-retardant polyurethane sealant. The sealant consists of a component A and a component B; the component A consists of the following components in parts by weight: 60-70 parts of polyurethane prepolymer, 3-5 parts of stearic acid, 22-24 parts of silicon oxide with the granularity of not greater than 200 meshes, 12-14 parts of nano titanium pigment, 18-20 parts of zirconium dioxide with the granularity of not greater than 400 meshes, 6-8 parts of plasticizer, 12-14 parts of viscosity increaser, 3-5 parts of flame-retardant aluminum hydroxide, 5-7 parts of flame-retardant zinc borate and 6-8 parts of melamine chlorinated isocyanurates; the component B consists of the following components in parts by weight: 40-50 parts of manganese peroxide, 12-16 parts of plasticizer, 10-12 parts of tellurium dioxide, 7-9 parts of sodium di-n--butyl dithiocarbamate, 20-24 parts of kaolin and 22-26 parts of white carbon black; the mass ratio of the component A to the component B is (3-4):1. The preparation method comprises the following steps: 1) preparing a polyurethane prepolymer; 2), preparing the component A; and 3) preparing the component B.
Description
Technical field
The present invention relates to construction sealing materials field, particularly a kind of preparation method of high-strength fire-retarding polyurethane sealant.
Background technology
Silicane-modified polyurethane is a kind of type material, it has the advantage of urethane and organosilicon material simultaneously, there is the excellent properties such as wet-heat resisting, oil resistant, chemicals-resistant, wear-resisting, good preservation stability, be widely used in Europe in recent years preparing high-performance room-temperature vulcanizing sealant.Compared with conventional urethane sealing agent, silicane-modified polyurethane has obvious advantage in curing mechanism, performance and use: from curing mechanism, silicane-modified polyurethane is under the effect of catalyzer, the alkoxyl group of silane and moisture are hydrolyzed and condensation, form stable siloxanes (Si-O-Si) three-dimensional net structure, which overcome mono-component polyurethane to react by isocyano and moisture and solidify, reaction process forms the weakness of bubble because releasing carbonic acid gas; From make for, silicane-modified polyurethane do not need silane coupling agent just can with non-porous material surface strong bond.
Silicane-modified polyurethane self-strength is not high, and general tensile strength, less than 1MPa, if for the preparation of seal gum, must add reinforced filling, adds the performance such as physics, machinery that filler can increase material in seal gum.
The various things that run through that flame retardant sealant is mainly used in larger displacement are if cable, airduct, oil pipe, tracheae etc. are through the fire-resisting division of the various opening formed when wall, floor and cable testing bridge.But the most flame retardant sealant sticking power used at present and poor flexibility, to affect by extraneous factor and easily make flame retardant sealant and run through between thing or perforated wall to form gap as temperature variation, vibration etc. running through thing, cause fire prevention lost efficacy and needed again to change flame retardant sealant, expense is larger.As No. 03117403.5 Chinese patent, disclose one " neutral silicone fireproof seal gum and manufacture method thereof ", although its flame-proof silicone sealant can be fire-retardant, but swelling property is poor when meeting fire, if any when forming gap between penetration piece or perforated wall, fire protection flame retarding sealing effectiveness is bad, and production cost is higher.At present along with the raising that building safety requires, require that material of construction has good flame retardant resistance.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is the preparation method providing a kind of high-strength fire-retarding polyurethane sealant.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of preparation method of high-strength fire-retarding polyurethane sealant, described seal gum is made up of A, B component, represent with weight part, wherein component A is made up of following component: polyurethane prepolymer 60-70 part, stearic acid 3-5 part,-200 order silicon oxide 22-24 parts, nanometer titanium dioxide 12-14 part ,-400 order zirconium dioxide 18-20 parts, softening agent 6-8 part, tackifier 12-14 part, fire-retardant aluminium hydroxide 3-5 part, fire-retardant zinc borate 5-7 part, melamine cyanurate 6-8 part; B component is made up of following component: Manganse Dioxide 40-50 part, softening agent 12-16 part, tellurium dioxide 10-12 part, NB sodium dibutyl dithiocarbamate 7-9 part, kaolin 20-24 part, white carbon black 22-26 part; The weight proportion of described A, B component is A: B=3-4: 1, and described preparation method comprises the steps:
1) polyurethane preformed polymer: described polyurethane prepolymer is made up of according to 1: 1: 1 mixing terminal mercapto polyurethane fluid rubber, base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II tri-part; Described terminal mercapto polyurethane fluid rubber be with complete synthesis urethane be main chain, the fluid rubber of sulfydryl end-blocking, 25 DEG C of viscosity are 42.0 × 10
4-50.0 × 10
4mPas, sulfydryl mass percentage is 1.0-2.0%, mass percentage≤0.15% of residual isocyano; Biuret polyisocyanate and polyether glycol are reacted obtained at 105-110 DEG C by described base polyurethane prepolymer for use as I, and wherein the mass ratio of biuret polyisocyanate and polyether glycol is 30: 1; The polytetrahydrofuran diol of molecular mass between 6500-7500 and the polyoxytrimethylene triol of molecular mass between 8500-10000 mix by described base polyurethane prepolymer for use as II, the ratio of the two is 1: 3.5, at the temperature of 120 DEG C, under the vacuum that is less than 0.1MPa dry 1 hour, then be cooled to 75 DEG C and add the isocyanic ester accounting for said mixture mass percent 18% and the dibutyl tin laurate accounting for said mixture mass percent 0.2% again, react 3 hours, obtained polyurethane prepolymer II;
2) preparation of component A: join in kneader by the fire-retardant aluminium hydroxide in component A, fire-retardant zinc borate, melamine cyanurate and polyurethane prepolymer, is under the vacuum of 0.03-0.05MPa in vacuum tightness, stirs 60-90min under 1050-1100r/min stirring velocity; Then add stearic acid ,-200 order silicon oxide successively, nanometer titanium dioxide ,-400 order zirconium dioxides, softening agent, tackifier, be then reduced to 300-400r/min by stirring velocity, stirs 120-150min, extrude, obtain component A;
3) preparation of B component: each material in B component is joined in kneader successively, stirs 40-60min under 300-400r/min mixes speed, extrude, grind, obtain B component.
Wherein, described softening agent is any one or two kinds of in dibutyl phthalate, dioctyl phthalate (DOP), butyl benzyl phthalate, dihexyl phthalate, diisononyl phthalate;
Wherein, described tackifier are octyl group phenolic tackifying resins, Alkylphenolic Tackifying Resin, tertiary butyl phenolic tackifying resins, liquid-state epoxy resin, C
5any one in petroleum resin and liquid coumarone indene resin, or any two.
Beneficial effect of the present invention is:
1) assembly of the preferred basic glue of the present invention, the prepolymer of mixing three kinds of urethane, and allocate according to the ratio row of 1: 1: 1, play the respective advantage of three kinds of prepolymers, reach synergy, make the excellent combination property of basic glue, ensure that the realization of higher mechanical property, and provide good support for the fusion of fire retardant.
2) the present invention is by the optimization of filler in component A, selected silicon oxide, titanium dioxide and zirconium dioxide three kinds of components, three kinds of components are made to play different effects respectively, wherein silicon oxide improves gel strength, nano titanium oxide improves colloid whole synthesis performance, the far super micro-scale titanium dioxide of its effect, arrange in pairs or groups with fire retardant and can play cooperative flame retardant effect, zirconium dioxide improves the high temperature resistant attribute of colloid, it is made still to keep good flame retardant effect at relatively high temperatures, experiment shows that the granularity of three kinds of fillers has tremendous influence to colloidal property, non-nano titanium dioxide or-200 order silicon oxide or non-400 order zirconium dioxide is adopted all to cause the deterioration of performance.
3) the selected and basic glue fire retardant of arranging in pairs or groups, and respective content is determined on the basis of great many of experiments: fire-retardant aluminium hydroxide 3-5 part, fire-retardant zinc borate 5-7 part, melamine cyanurate 6-8 part, seal gum prepared by the present invention fire prevention index all reaches the technical requirements of GA161-1997 " performance requriements of fire-proof sealing material and experimental technique ".
4) the permanent sealing that the sealing glue solidifying postadhesion power prepared of the present invention is strong, good springiness, good airproof performance, weather resisteant are good, can keep seam.
5) seal gum of the present invention is to environment and body harmless, is a kind of environmentally friendly machine.
Embodiment
Softening agent in following examples one to three is any one or two kinds of in dibutyl phthalate, dioctyl phthalate (DOP), butyl benzyl phthalate, dihexyl phthalate, diisononyl phthalate; Tackifier are octyl group phenolic tackifying resins, Alkylphenolic Tackifying Resin, tertiary butyl phenolic tackifying resins, liquid-state epoxy resin, C
5any one in petroleum resin and liquid coumarone indene resin, or any two.
Embodiment one
A kind of preparation method of high-strength fire-retarding polyurethane sealant, described seal gum is made up of A, B component, represent with weight part, wherein component A is made up of following component: polyurethane prepolymer 60 parts, stearic acid 5 parts,-200 order silicon oxide 22 parts, nanometer titanium dioxide 14 parts ,-400 order zirconium dioxides 18 parts, 8 parts, softening agent, tackifier 12 parts, 5 parts, fire-retardant aluminium hydroxide, fire-retardant zinc borate 5 parts, melamine cyanurate 8 parts; B component is made up of following component: Manganse Dioxide 40 parts, 16 parts, softening agent, tellurium dioxide 10 parts, NB sodium dibutyl dithiocarbamate 9 parts, kaolin 20 parts, white carbon black 26 parts; The weight proportion of described A, B component is A: B=3: 1, and described preparation method comprises the steps:
1) polyurethane preformed polymer: described polyurethane prepolymer is made up of according to 1: 1: 1 mixing terminal mercapto polyurethane fluid rubber, base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II tri-part; Described terminal mercapto polyurethane fluid rubber be with complete synthesis urethane be main chain, the fluid rubber of sulfydryl end-blocking, 25 DEG C of viscosity are 42.0 × 10
4-50.0 × 10
4mPas, sulfydryl mass percentage is 1.0-2.0%, mass percentage≤0.15% of residual isocyano; Biuret polyisocyanate and polyether glycol are reacted obtained at 105-110 DEG C by described base polyurethane prepolymer for use as I, and wherein the mass ratio of biuret polyisocyanate and polyether glycol is 30: 1; The polytetrahydrofuran diol of molecular mass between 6500-7500 and the polyoxytrimethylene triol of molecular mass between 8500-10000 mix by described base polyurethane prepolymer for use as II, the ratio of the two is 1: 3.5, at the temperature of 120 DEG C, under the vacuum that is less than 0.1MPa dry 1 hour, then be cooled to 75 DEG C and add the isocyanic ester accounting for said mixture mass percent 18% and the dibutyl tin laurate accounting for said mixture mass percent 0.2% again, react 3 hours, obtained polyurethane prepolymer II;
2) preparation of component A: join in kneader by the fire-retardant aluminium hydroxide in component A, fire-retardant zinc borate, melamine cyanurate and polyurethane prepolymer, is under the vacuum of 0.03MPa in vacuum tightness, stirs 60min under 1100r/min stirring velocity; Then add stearic acid ,-200 order silicon oxide successively, nanometer titanium dioxide ,-400 order zirconium dioxides, softening agent, tackifier, be then reduced to 400r/min by stirring velocity, stirs 120min, extrude, obtain component A;
3) preparation of B component: each material in B component is joined in kneader successively, stirs 60min under 300r/min mixes speed, extrude, grind, obtain B component.
Embodiment two
A kind of preparation method of high-strength fire-retarding polyurethane sealant, described seal gum is made up of A, B component, represent with weight part, wherein component A is made up of following component: polyurethane prepolymer 70 parts, stearic acid 3 parts,-200 order silicon oxide 24 parts, nanometer titanium dioxide 12 parts ,-400 order zirconium dioxides 20 parts, 6 parts, softening agent, tackifier 14 parts, 3 parts, fire-retardant aluminium hydroxide, fire-retardant zinc borate 7 parts, melamine cyanurate 6 parts; B component is made up of following component: Manganse Dioxide 50 parts, 12 parts, softening agent, tellurium dioxide 12 parts, NB sodium dibutyl dithiocarbamate 7 parts, kaolin 24 parts, white carbon black 22 parts; The weight proportion of described A, B component is A: B=4: 1, and described preparation method comprises the steps:
1) polyurethane preformed polymer: described polyurethane prepolymer is made up of according to 1: 1: 1 mixing terminal mercapto polyurethane fluid rubber, base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II tri-part; Described terminal mercapto polyurethane fluid rubber be with complete synthesis urethane be main chain, the fluid rubber of sulfydryl end-blocking, 25 DEG C of viscosity are 42.0 × 10
4-50.0 × 10
4mPas, sulfydryl mass percentage is 1.0-2.0%, mass percentage≤0.15% of residual isocyano; Biuret polyisocyanate and polyether glycol are reacted obtained at 105-110 DEG C by described base polyurethane prepolymer for use as I, and wherein the mass ratio of biuret polyisocyanate and polyether glycol is 30: 1; The polytetrahydrofuran diol of molecular mass between 6500-7500 and the polyoxytrimethylene triol of molecular mass between 8500-10000 mix by described base polyurethane prepolymer for use as II, the ratio of the two is 1: 3.5, at the temperature of 120 DEG C, under the vacuum that is less than 0.1MPa dry 1 hour, then be cooled to 75 DEG C and add the isocyanic ester accounting for said mixture mass percent 18% and the dibutyl tin laurate accounting for said mixture mass percent 0.2% again, react 3 hours, obtained polyurethane prepolymer II;
2) preparation of component A: join in kneader by the fire-retardant aluminium hydroxide in component A, fire-retardant zinc borate, melamine cyanurate and polyurethane prepolymer, is under the vacuum of 0.05MPa in vacuum tightness, stirs 90min under 1050r/min stirring velocity; Then add stearic acid ,-200 order silicon oxide successively, nanometer titanium dioxide ,-400 order zirconium dioxides, softening agent, tackifier, be then reduced to 300r/min by stirring velocity, stirs 150min, extrude, obtain component A;
3) preparation of B component: each material in B component is joined in kneader successively, stirs 40min under 400r/min mixes speed, extrude, grind, obtain B component.
Embodiment three
A kind of preparation method of high-strength fire-retarding polyurethane sealant, described seal gum is made up of A, B component, represent with weight part, wherein component A is made up of following component: polyurethane prepolymer 65 parts, stearic acid 4 parts,-200 order silicon oxide 23 parts, nanometer titanium dioxide 13 parts ,-400 order zirconium dioxides 19 parts, 7 parts, softening agent, tackifier 13 parts, 4 parts, fire-retardant aluminium hydroxide, fire-retardant zinc borate 6 parts, melamine cyanurate 7 parts; B component is made up of following component: Manganse Dioxide 45 parts, 14 parts, softening agent, tellurium dioxide 11 parts, NB sodium dibutyl dithiocarbamate 8 parts, kaolin 22 parts, white carbon black 24 parts; The weight proportion of described A, B component is A: B=3.5: 1, and described preparation method comprises the steps:
1) polyurethane preformed polymer: described polyurethane prepolymer is made up of according to 1: 1: 1 mixing terminal mercapto polyurethane fluid rubber, base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II tri-part; Described terminal mercapto polyurethane fluid rubber be with complete synthesis urethane be main chain, the fluid rubber of sulfydryl end-blocking, 25 DEG C of viscosity are 42.0 × 10
4-50.0 × 10
4mPas, sulfydryl mass percentage is 1.0-2.0%, mass percentage≤0.15% of residual isocyano; Biuret polyisocyanate and polyether glycol are reacted obtained at 105-110 DEG C by described base polyurethane prepolymer for use as I, and wherein the mass ratio of biuret polyisocyanate and polyether glycol is 30: 1; The polytetrahydrofuran diol of molecular mass between 6500-7500 and the polyoxytrimethylene triol of molecular mass between 8500-10000 mix by described base polyurethane prepolymer for use as II, the ratio of the two is 1: 3.5, at the temperature of 120 DEG C, under the vacuum that is less than 0.1MPa dry 1 hour, then be cooled to 75 DEG C and add the isocyanic ester accounting for said mixture mass percent 18% and the dibutyl tin laurate accounting for said mixture mass percent 0.2% again, react 3 hours, obtained polyurethane prepolymer II;
2) preparation of component A: join in kneader by the fire-retardant aluminium hydroxide in component A, fire-retardant zinc borate, melamine cyanurate and polyurethane prepolymer, is under the vacuum of 0.04MPa in vacuum tightness, stirs 75min under 1080r/min stirring velocity; Then add stearic acid ,-200 order silicon oxide successively, nanometer titanium dioxide ,-400 order zirconium dioxides, softening agent, tackifier, be then reduced to 350r/min by stirring velocity, stirs 135min, extrude, obtain component A;
3) preparation of B component: each material in B component is joined in kneader successively, stirs 50min under 350r/min mixes speed, extrude, grind, obtain B component.
The performance of seal gum prepared by above-described embodiment one to three is as follows:
| Project | Standard | Embodiment one | Embodiment two | Embodiment three |
| Flame retardant resistance | FV-0 | FV-0 | FV-0 | |
| Surface drying time | ≤24h | 2 | 1.5 | 1.2 |
| Sag | ≤3mm | 1 | 0.5 | 0 |
| Extrudability | ≥80ml/min | 180 | 170 | 200 |
| 23 DEG C of tensile moduluses | ＞0.4MPa | 2.7 | 2.5 | 3.2 |
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (3)
1. the preparation method of a high-strength fire-retarding polyurethane sealant, it is characterized in that, described seal gum is made up of A, B component, represent with weight part, wherein component A is made up of following component: polyurethane prepolymer 60-70 part, stearic acid 3-5 part ,-200 order silicon oxide 22-24 parts, nanometer titanium dioxide 12-14 part ,-400 order zirconium dioxide 18-20 parts, softening agent 6-8 part, tackifier 12-14 part, fire-retardant aluminium hydroxide 3-5 part, fire-retardant zinc borate 5-7 part, melamine cyanurate 6-8 part; B component is made up of following component: Manganse Dioxide 40-50 part, softening agent 12-16 part, tellurium dioxide 10-12 part, NB sodium dibutyl dithiocarbamate 7-9 part, kaolin 20-24 part, white carbon black 22-26 part; The weight proportion of described A, B component is A: B=3-4: 1, and described preparation method comprises the steps:
1) polyurethane preformed polymer: described polyurethane prepolymer is made up of according to 1: 1: 1 mixing terminal mercapto polyurethane fluid rubber, base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II tri-part; Described terminal mercapto polyurethane fluid rubber be with complete synthesis urethane be main chain, the fluid rubber of sulfydryl end-blocking, 25 DEG C of viscosity are 42.0 × 10
4-50.0 × 10
4mPas, sulfydryl mass percentage is 1.0-2.0%, mass percentage≤0.15% of residual isocyano; Biuret polyisocyanate and polyether glycol are reacted obtained at 105-110 DEG C by described base polyurethane prepolymer for use as I, and wherein the mass ratio of biuret polyisocyanate and polyether glycol is 30: 1; The polytetrahydrofuran diol of molecular mass between 6500-7500 and the polyoxytrimethylene triol of molecular mass between 8500-10000 mix by described base polyurethane prepolymer for use as II, the ratio of the two is 1: 3.5, at the temperature of 120 DEG C, under the vacuum that is less than 0.1MPa dry 1 hour, then be cooled to 75 DEG C and add the isocyanic ester accounting for said mixture mass percent 18% and the dibutyl tin laurate accounting for said mixture mass percent 0.2% again, react 3 hours, obtained polyurethane prepolymer II;
2) preparation of component A: join in kneader by the fire-retardant aluminium hydroxide in component A, fire-retardant zinc borate, melamine cyanurate and polyurethane prepolymer, is under the vacuum of 0.03-0.05MPa in vacuum tightness, stirs 60-90min under 1050-1100r/min stirring velocity; Then add stearic acid ,-200 order silicon oxide successively, nanometer titanium dioxide ,-400 order zirconium dioxides, softening agent, tackifier, be then reduced to 300-400r/min by stirring velocity, stirs 120-150min, extrude, obtain component A;
3) preparation of B component: each material in B component is joined in kneader successively, stirs 40-60min under 300-400r/min mixes speed, extrude, grind, obtain B component.
2. the preparation method of a kind of high-strength fire-retarding polyurethane sealant as claimed in claim 1, it is characterized in that, described softening agent is any one or two kinds of in dibutyl phthalate, dioctyl phthalate (DOP), butyl benzyl phthalate, dihexyl phthalate, diisononyl phthalate.
3. the preparation method of a kind of high-strength fire-retarding polyurethane sealant as described in claim 1-2, is characterized in that, described tackifier are octyl group phenolic tackifying resins, Alkylphenolic Tackifying Resin, tertiary butyl phenolic tackifying resins, liquid-state epoxy resin, C
5any one in petroleum resin and liquid coumarone indene resin, or any two.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527280A (en) * | 2019-09-27 | 2019-12-03 | 南京瑞兴科技有限公司 | A kind of roofing extruded sheet envelope painting material |
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| US6043304A (en) * | 1995-11-09 | 2000-03-28 | Raychem Limited | Flame-retarded adhesive composition |
| CN101402845A (en) * | 2008-11-11 | 2009-04-08 | 北京市化学工业研究院 | Process for producing flame-proof fluid sealant for construction |
| CN101434825A (en) * | 2008-12-12 | 2009-05-20 | 河南永丽化工有限公司 | Bicomponent terminal mercapto polyurethane mildewproof sealant and preparation thereof |
| CN104531040A (en) * | 2014-10-09 | 2015-04-22 | 广东新展化工新材料有限公司 | Polyurethane acrylate sealant and preparation method thereof |
-
2015
- 2015-05-29 CN CN201510287516.3A patent/CN104893641A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6043304A (en) * | 1995-11-09 | 2000-03-28 | Raychem Limited | Flame-retarded adhesive composition |
| CN101402845A (en) * | 2008-11-11 | 2009-04-08 | 北京市化学工业研究院 | Process for producing flame-proof fluid sealant for construction |
| CN101434825A (en) * | 2008-12-12 | 2009-05-20 | 河南永丽化工有限公司 | Bicomponent terminal mercapto polyurethane mildewproof sealant and preparation thereof |
| CN104531040A (en) * | 2014-10-09 | 2015-04-22 | 广东新展化工新材料有限公司 | Polyurethane acrylate sealant and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527280A (en) * | 2019-09-27 | 2019-12-03 | 南京瑞兴科技有限公司 | A kind of roofing extruded sheet envelope painting material |
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Application publication date: 20150909 |