CN101302420A - High-expansion fireproof sealant and preparation thereof - Google Patents
High-expansion fireproof sealant and preparation thereof Download PDFInfo
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- CN101302420A CN101302420A CNA2008100454314A CN200810045431A CN101302420A CN 101302420 A CN101302420 A CN 101302420A CN A2008100454314 A CNA2008100454314 A CN A2008100454314A CN 200810045431 A CN200810045431 A CN 200810045431A CN 101302420 A CN101302420 A CN 101302420A
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Abstract
The invention discloses high intumescent fire stopping mastic and a method for preparing the same. The mastic is prepared by taking acrylate emulsion (or elastic styrene-acrylate emulsion), polybutene (or polyisobutylene), glycol, emulsifying agent and tritolyl phosphate as base materials with addition of certain auxiliary materials. The preparation method is as follows: the base materials are added into a reaction kettle according to certain mass portion, stirred, slowly heated and insulated for a period of time, and transferred into a colloid stirrer; auxiliary materials such as ammonium polyphosphates, flame-retarding aluminum hydroxide, flame-retarding zinc borates, calcium carbonates, expandable graphite, iron oxide red and glass fibers are gradually added into the mixture under the condition of stirring; and the process of stirring is continued until a colloid is uniform. The fire stopping mastic prepared by adoption of the method can be quickly carbonized and expanded to 5 to 8 times of the prior volume in case of fire, and can not fall off; the strength and the heat insulation after solidification are good, and the fire resistance is very good; and the adhesion is strong and the elasticity is good. The high intumescent fire stopping mastic and the method are particularly suitable for fire compartmentation of various penetrating penetration assemblies such as cables, cable bridges, pipes and so on.
Description
Technical field
The present invention relates to a kind of polymer fire-proof sealing material and preparation method thereof, specifically is a kind of high-expansion fireproof sealant and preparation method thereof.
Background technology
Fire-proof sealing material (fireproof seal gum) is mainly used in the various openings that form when various penetration pieces such as cable, airduct, oil pipe, tracheae etc. pass wall, floor and the fire-resisting division of cable testing bridge.
Present fireproof seal gum and manufacture method thereof are more, but most fire-proof sealing material sticking power and elasticity are relatively poor, influenced as temperature variation, vibration etc. by extraneous factor at penetration piece, easily make between fire-proof sealing material and penetration piece or perforated wall and form the slit, cause the fire prevention inefficacy and need change plugging material again, expense is bigger.As No. 03117403.5 Chinese patent, disclose a kind of " neutral silicone fireproof seal gum and manufacture method thereof ", although its flame-proof silicone sealant can be fire-retardant, swelling property is relatively poor when meeting fire, when forming the slit between penetration piece or perforated wall, the fire protection flame retarding sealing effectiveness is bad; No. 200610039175.9 Chinese patents and for example; a kind of " expansion fire-proof adhesive " disclosed; in its component just like the composition of expandable flame retardants such as expanded graphite; fire-retardant expansion effect is better when meeting fire; but lack the protection to expansion charcoal layer such as glass fibre in the component; easily produce loose expansion charcoal layer when catching fire, expansion charcoal layer easily comes off when expanding volume is excessive.And the preparation technology of these seal gums is complicated, production cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of high-expansion fireproof sealant and preparation method thereof.
The present invention is achieved in that
A kind of high-expansion fireproof sealant comprises base-material and auxiliary material, contains ammonium polyphosphate, expanded graphite in the auxiliary material, it is characterized in that: the base-material of described seal gum is acrylic ester emulsion, polybutene, ethylene glycol, emulsifying agent and Tritolyl Phosphate; Also contain fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, red iron oxide and glass fibre in the auxiliary material.
The base-material of described seal gum can also be phenylpropyl alcohol elastic emulsion, polyisobutene, ethylene glycol, emulsifying agent and Tritolyl Phosphate; Also contain fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, red iron oxide and glass fibre in the auxiliary material.
Described emulsifying agent is sodium lauryl sulphate and/or OP-10, and the name of OP-10 is called the alkylphenol polyvinyl ether.
The recipe ingredient of described seal gum is by weight:
100 parts of acrylic ester emulsions (or phenylpropyl alcohol elastic emulsion);
5～15 parts of polybutene (or polyisobutene);
2～5 parts of ethylene glycol;
8～12 parts of Tritolyl Phosphates;
2～4 parts of emulsifying agents (sodium lauryl sulphate or OP-10);
30～50 parts of ammonium polyphosphates;
40～60 parts in lime carbonate;
15～30 parts in fire-retardant aluminium hydroxide;
2～4 parts of zinc borates;
3～4 parts of red iron oxides;
8～16 parts of expanded graphites;
3～6 parts in glass fibre.
The second-order transition temperature (Tg) of described acrylic ester emulsion (or phenylpropyl alcohol elastic emulsion) is-20～5 ℃, solid content 50%, viscosity 100～500mPa.s; The molecular weight of polybutene (or polyisobutene) is 10000～20000.
A kind of preparation method of high-expansion fireproof sealant is characterized in that: the preparation method of described fireproof seal gum such as following steps:
(1) with acrylic ester emulsion (or phenylpropyl alcohol elastic emulsion), polybutene (or polyisobutene), ethylene glycol, Tritolyl Phosphate and emulsifying agent, in the mass fraction adding reactor by described prescription, under agitation slowly to heat, be incubated, cooling obtains base-material;
(2) base-material is changed in the colloid agitator, under agitation condition, add the ammonium polyphosphate of described prescription quality umber, fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, expanded graphite, red iron oxide and glass fibre gradually, continue to be stirred to colloid and evenly get final product.
Its supplementary features are: the base-material Heating temperature in the described step (1) is 50～80 ℃; Soaking time 60～120min; The reinforced time of continuing to stir is 1～2 hour in the described step (2).
Effect of the present invention is: the high-expansion fireproof sealant that adopts method preparation of the present invention, owing to be base-material in the component of seal gum with water-soluble poly butylene modification acrylate (elasticity) emulsion, little, the good springiness of back volumetric shrinkage is solidified in organic solvent-free volatilization in use; Strong adhesion, good airproof performance; And intensity, heat insulation, flame retardant resistance is fabulous, can keep the permanent sealing of penetration piece and parietal suture.Fireproof seal gum of the present invention meets rapidly charing of fire under natural situation, be expanded to 5～8 times of original volume, and charring layer does not come off, even also can be full of rapidly and seal in bigger hole with the seal failure of penetration piece and parietal suture, when catching fire under the influences such as the energy assurance is of a specified duration in extraneous factor such as year, temperature variation, vibration, reach purpose fire-retardant, fire insulation fully, thereby be specially adapted to the fire-resisting division of various penetration pieces such as cable, cable testing bridge and pipeline.
Embodiment
Fireproof seal gum of the present invention is made up of base-material and auxiliary material, and base-material is acrylic ester emulsion (or phenylpropyl alcohol elastic emulsion), polybutene (or polyisobutene), ethylene glycol, emulsifying agent and Tritolyl Phosphate; Auxiliary material is ammonium polyphosphate, fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, expanded graphite, red iron oxide and glass fibre; Its recipe ingredient is by weight:
100 parts of acrylic ester emulsions (or phenylpropyl alcohol elastic emulsion), Tg is-20～5 ℃, solid content 50%, viscosity 100～500mPa..s;
5～15 parts of polybutene (or polyisobutene), molecular weight 10000～20000;
8～12 parts of Tritolyl Phosphates;
2～5 parts of ethylene glycol;
2～4 parts of emulsifying agents (sodium lauryl sulphate or OP-10);
30～50 parts of ammonium polyphosphates, the polymerization degree be greater than 1000, 〉=1200 orders;
40～60 parts in lime carbonate, 〉=1500 orders;
15～30 parts in fire-retardant aluminium hydroxide, 〉=1200 orders;
2～4 parts of zinc borates;
3～4 parts of red iron oxides;
8～16 parts of expanded graphites, 100～200ml/g, pH5～7;
3～6 parts in glass fibre, 3～5mm, diameter 5～10 μ m.
Preparation method of the present invention is as follows:
1. with acrylic ester emulsion (or phenylpropyl alcohol elastic emulsion), polybutene (or polyisobutene), ethylene glycol, Tritolyl Phosphate and emulsifying agent, mass fraction by described prescription adds in the reactor, under agitation slowly be heated to 50 ℃～80 ℃, insulation 60min～120min, cooling obtains base-material;
2. base-material is changed in the colloid agitator, under agitation condition, add the ammonium polyphosphate of described prescription quality umber, fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, expanded graphite, ferric oxide and glass fibre gradually, continue to stir and evenly to get final product to colloid in 1～2 hour.
Embodiment 1
1. get 100 parts of acrylic ester elastic emulsions, 12 parts of Tritolyl Phosphates, 2 parts of ethylene glycol, 15 parts of polybutene, each 1 part of emulsifying agent (sodium lauryl sulphate, OP-10), add in the reactor, under agitation slowly be heated to 50 ℃, insulation 60min, cooling obtains base-material;
2. base-material is changed in the colloid agitator, under agitation condition, add 4 parts in 30 parts of ammonium polyphosphates, 40 parts in lime carbonate, 30 parts in fire-retardant aluminium hydroxide, 2 parts of zinc borates, 4 parts of red iron oxides, 16 parts of expanded graphites and glass fibre gradually, continue to stir and evenly got final product to colloid in 1 hour.
Embodiment 2
1. get 100 parts of acrylic ester elastic emulsions, 8 parts of Tritolyl Phosphates, 5 parts of ethylene glycol, 5 parts of polybutene, 3 parts of emulsifying agents (sodium lauryl sulphate), add in the reactor, under agitation slowly be heated to 60 ℃, insulation 80min, cooling obtains base-material;
2. base-material is changed in the colloid agitator, under agitation condition, add 6 parts in 40 parts of ammonium polyphosphates, 50 parts in lime carbonate, 20 parts in fire-retardant aluminium hydroxide, 4 parts of zinc borates, 4 parts of red iron oxides, 12 parts of expanded graphites and glass fibre gradually, continue to stir and evenly got final product to colloid in 1.5 hours.
Embodiment 3
1. get 100 parts of phenylpropyl alcohol elastic emulsions, 10 parts of Tritolyl Phosphates, 3 parts of ethylene glycol, 10 parts of polyisobutene, 4 parts of emulsifying agents (OP-10), add in the reactor, under agitation slowly be heated to 80 ℃, insulation 120min, cooling obtains base-material;
2. base-material is changed in the colloid agitator, under agitation condition, add 3 parts in 50 parts of ammonium polyphosphates, 60 parts in lime carbonate, 15 parts in fire-retardant aluminium hydroxide, 3 parts of zinc borates, 3 parts of red iron oxides, 8 parts of expanded graphites and glass fibre gradually, continue to stir and evenly got final product to colloid in 2 hours.
Fireproof seal gum of the present invention has elasticity and sticking power preferably, and stretching displacement amount 5%～10% depends on the moisture in envrionment temperature and the colloid its set time, and it is little to solidify volumetric shrinkage, but appearance brushing paint etc., use temperature-10 ℃～80 ℃.Press GB161-1997 " performance requriements of fire-proof sealing material and experimental technique ", with cable, steel pipe (penetration piece) is example, expansion fireproof sealant of the present invention is carried out the detection of fire-resistant experiment, the temperature rise of each point for measuring temperature much smaller than standard-required 180 (℃), peak temperature rise only 105 (℃), lowest temperature rise 21 (℃), average temperature rising 54 (℃), so the fire performance of seal gum is fabulous, the requirement of conformance with standard regulation fully.Its fire-resistant detection case such as following table:
The fire performance of table 1 expansion fireproof sealant detects index
| Time (min) | Point for measuring temperature 1 (℃) | Point for measuring temperature 2 (℃) | Point for measuring temperature 3 (℃) | Point for measuring temperature 4 (℃) | Point for measuring temperature 5 (℃) | Temperature in the stove (℃) |
| 90 | 108 | 110 | 34 | 32 | 45 | 1030 |
| 120 | 115 | 116 | 37 | 37 | 47 | 1089 |
| 150 | 123 | 121 | 45 | 41 | 45 | 1109 |
| 183 | 128 | 127 | 45 | 44 | 45 | 1109 |
The physical and chemical index of the close expansible fireproof sealing of table 2
| Sequence number | Project | Standard index | The actual measurement index | Detected result |
| 1 | Outward appearance | Plastic solidification has certain snappiness | The red plastic solid has snappiness | Meet |
| 2 | Density (Kg/m 3) | ≤2.0×10 3 | 1.5～1.6×10 3 | Meet |
| 3 | Water tolerance, d 〉= | 3, no swelling, cracking | 3, no swelling, cracking | Meet |
| 4 | Oil-proofness, d 〉= | 3, no swelling, cracking | 3, no swelling, cracking | Meet |
| 5 | Solidity to corrosion, d 〉= | 7, non-corroding, corrosion phenomenon | 7, non-corroding, corrosion phenomenon | Meet |
Claims (7)
1. a high-expansion fireproof sealant comprises base-material and auxiliary material, contains ammonium polyphosphate, expanded graphite in the auxiliary material, it is characterized in that: the base-material of described seal gum is acrylic ester emulsion, polybutene, ethylene glycol, emulsifying agent and Tritolyl Phosphate; Also contain fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, red iron oxide and glass fibre in the auxiliary material.
2. according to the described high-expansion fireproof sealant of claim 1, it is characterized in that: the base-material of described seal gum is phenylpropyl alcohol elastic emulsion, polyisobutene, ethylene glycol, emulsifying agent and Tritolyl Phosphate; Also contain fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, red iron oxide and glass fibre in the auxiliary material.
3. according to claim 1 or 2 described high-expansion fireproof sealants, it is characterized in that: described emulsifying agent is sodium lauryl sulphate and/or OP-10.
4. according to claim 1 or 2 or 3 described high-expansion fireproof sealants, it is characterized in that: the recipe ingredient of described seal gum is by weight:
100 parts of acrylic ester emulsions (or phenylpropyl alcohol elastic emulsion);
5～15 parts of polybutene (or polyisobutene);
2～5 parts of ethylene glycol;
8～12 parts of Tritolyl Phosphates;
2～4 parts of emulsifying agents (sodium lauryl sulphate or OP-10);
30～50 parts of ammonium polyphosphates;
40～60 parts in lime carbonate;
15～30 parts in fire-retardant aluminium hydroxide;
2～4 parts of zinc borates;
3～4 parts of red iron oxides;
8～16 parts of expanded graphites;
3～6 parts in glass fibre.
5. according to the described high-expansion fireproof sealant of claim 4, it is characterized in that: the second-order transition temperature (Tg) of described acrylic ester emulsion (or phenylpropyl alcohol elastic emulsion) is-20～5 ℃, solid content 50%, viscosity 100～500mPa.s; The molecular weight of polybutene (or polyisobutene) is 10000～20000.
6. according to the preparation method of claim 1 or 2 or 5 described high-expansion fireproof sealants, it is characterized in that: the preparation method of described fireproof seal gum such as following steps:
(1) with acrylic ester emulsion (or phenylpropyl alcohol elastic emulsion), polybutene (or polyisobutene), ethylene glycol, Tritolyl Phosphate and emulsifying agent, in the mass fraction adding reactor by described prescription, under agitation slowly to heat, be incubated, cooling obtains base-material;
(2) base-material is changed in the colloid agitator, under agitation condition, add the ammonium polyphosphate of described prescription quality umber, fire-retardant aluminium hydroxide, fire-retardant zinc borate, lime carbonate, expanded graphite, red iron oxide and glass fibre gradually, continue to be stirred to colloid and evenly get final product.
7. by the preparation method of the described high-expansion fireproof sealant of claim 6, it is characterized in that: the base-material Heating temperature in the described step (1) is 50～80 ℃; Soaking time 60～120min; The reinforced time of continuing to stir is 1～2 hour in the described step (2).
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| CN2008100454314A CN101302420B (en) | 2008-07-01 | 2008-07-01 | High-expansion fireproof sealant and preparation thereof |
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| Publication Number | Publication Date |
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| CN101302420A true CN101302420A (en) | 2008-11-12 |
| CN101302420B CN101302420B (en) | 2010-12-29 |
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