CN1990928B - Halogen free flame-proof felt and its preparation method - Google Patents
Halogen free flame-proof felt and its preparation method Download PDFInfo
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- CN1990928B CN1990928B CN2005101120069A CN200510112006A CN1990928B CN 1990928 B CN1990928 B CN 1990928B CN 2005101120069 A CN2005101120069 A CN 2005101120069A CN 200510112006 A CN200510112006 A CN 200510112006A CN 1990928 B CN1990928 B CN 1990928B
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Abstract
The invention provides a mixture for producing non-halogen flame retardant felt, comprising (a) fiber with 30-80wt% of the total weight of mixture; (b) non-halogen flame retardant agent with 10-60wt% of the total weight of mixture; (c) adhesive agent with 10-50wt% of the total weight of mixture. The invention also provides a manufacturing method for said non-halogen flame retardant felt. The flame retardant felt in invention is provided with good flame retardant effect, low dissociating ammonia amount and low halogen amount, and can lessen the corrosion to metal part.
Description
Technical field
The present invention relates to a kind of fire prevention articles for use and preparation method thereof, relate to a kind of halogen free flame-proof felt and preparation method thereof particularly.
Background technology
That fire retardant felt has is heat insulation, insulation, sound-absorbing effect, can be widely used in automotive upholstery, compressor of air conditioner and other need the electrical and electronic component and the equipment of heat-insulating flame-retardant.In recent years, along with the consumption of fire retardant felt Application Areas constantly increases, to the fire-retardant requirement of felt and contain Dust Capacity, the requirement that contains aspects such as free ammonia amount is also more and more stricter.Because the fire retardant felt overwhelming majority is applied to electronic and electrical equipment, therefore need consider the etching problem of the metallic element in the equipment especially.For example, most of part is made by the copper metal material in the compressor of air conditioner, and the performance of fire retardant felt has also been proposed more strict requirement.
On the one hand, in existing fire retardant felt, normally by phenolic resins as bonding agent, re-use six methylene tetramines and make curing agent and come the cured flame-retardant felt.Contain ammonia in six methylene tetramines, so the contained free ammonia content of fire retardant felt is higher, thereby can causes corrosion the copper metal material.
On the other hand, if used fire retardant is halogen-containing, the fire retardant felt of Halogen incombustible agent and be heated and produce halide ion through long duration of action also can the corroding metal parts then, especially this corrosion situation is even more serious under high humidity, and Halogen is that the fire retardant felt of incombustible agent also can generate mordant hydrogen halide when discarded burning disposal.Therefore, the fire retardant of the nitrogenous element of Halogen need not as far as possible.
In addition, further simplify the production technology of fire retardant felt and reduce energy resource consumption and also become the task of top priority.
JP 07-003594 then introduced with powdery combustion inhibitor such as phosphoric acid, polyphosphoric acid, phosphate, etc. with after the waste and old fibre material evenly mixes, obtain the felt of a uniform thickness through shredding, frizzled feather, make the fusing of phenolic resins bonding agent, six methylene methylamines just can directly obtain fire retardant felt through heating again, but the easy moisture absorption of obtained flame-retardant felt, so poor water resistance, the ammon amount height.
In GB2227500, propose to adopt and resin adhesive such as polyvinyl chloride or polyvinyl acetate and fire retardant such as pollopas mixed and be made into slurries the felt processing of spraying, dried by hot-air oven or infrared heater then, but this technology obtained flame-retardant felt flame retardant effect is poor, can't reach flame retardant rating UL94 HF-1.
In sum, this area lacks and a kind ofly to possess good flame retardant effect and can reduce fire retardant felt to the corrosion of metal parts simultaneously again.Therefore this area presses for the exploitation good flame retardation effect, free ammon amount is low, halogen amount is low, reduce fire retardant felt to the corrosion of metal parts and preparation method thereof.
Summary of the invention
The objective of the invention is to obtain good flame retardation effect, free ammon amount is low, halogen amount is low, reduce fire retardant felt to the corrosion of metal parts and preparation method thereof
In a first aspect of the present invention, a kind of mixture that is used to prepare halogen free flame-proof felt is provided, described mixture comprises following component: (a) in the fiber of mixture total weight amount 30-80wt%; (b) in the halogen-free flame retardants of mixture total weight amount 10-60wt%; (c) in the bonding agent of mixture total weight amount 10-50wt%; Wherein, described fiber comprises natural fabric, synthetic fiber or its combination; Described halogen-free flame retardants is salt or its combination that inorganic acid and the metal that is selected from aluminium, calcium, magnesium, zinc form, and wherein said inorganic acid is selected from phosphoric acid, sulfuric acid, boric acid or its combination; Described bonding agent comprises thermoplastic resin, thermosetting resin or its combination.
In a preference of the present invention, the natural fabric that comprises in the described fiber is selected from cotton, hair, fiber crops or its combination; Described synthetic fiber are selected from viscose, polyester fiber, acrylic fibers, polyvinyl chloride fibre, polypropylene fibre or its combination.
In a preference of the present invention, described halogen-free flame retardants is selected from aluminium dihydrogen phosphate, calcium dihydrogen phosphate, calcium phosphate, magnesium phosphate, aluminum sulfate, wollastonite, Firebrake ZB or its combination.
In a preference of the present invention, described halogen-free flame retardants comprises in the dihydric phosphate of halogen-free flame retardants gross weight 50-70wt%, in the neutral salt of halogen-free flame retardants gross weight 30-50wt%, described dihydric phosphate comprises aluminium dihydrogen phosphate, calcium dihydrogen phosphate or its combination, and wherein said neutral salt comprises calcium phosphate, magnesium phosphate, aluminum sulfate, wollastonite, Firebrake ZB or its combination.
In a preference of the present invention, described thermoplastic resin is selected from polyvinyl chloride, polyvinyl acetate, ethylene-vinyl acetate copolymer, polyamide or its copolymer, polyethylene, polypropylene or its combination; Described thermosetting resin is selected from melamino-formaldehyde resin, Lauxite, phenolic resins or its combination.
In a preference of the present invention, described halogen-free flame retardants comprises in the aluminium dihydrogen phosphate of halogen-free flame retardants gross weight 50-70wt%, in the Firebrake ZB of halogen-free flame retardants gross weight 30-50wt%, and described bonding agent comprises in acetate-acetate ethylene copolymer of bonding agent gross weight 60-80wt%, in the Lauxite of bonding agent gross weight 20-40wt%; Perhaps described bonding agent comprises polyvinyl acetate in bonding agent gross weight 60-80wt%, in the melamino-formaldehyde resin of bonding agent gross weight 20-40wt%.
In a preference of the present invention, described halogen-free flame retardants is the powder of granularity between 2--200 μ m.
The present invention also provides a kind of method for preparing halogen free flame-proof felt, comprise the steps: (i) with (a) fiber, (b) halogen-free flame retardants and (c) bonding agent mix, form mixture, wherein said (a) fiber accounts for the 30-80wt% of mixture total weight amount, described (b) halogen-free flame retardants accounts for the 10-60wt% of mixture total weight amount, and described (c) bonding agent accounts for the 10-50wt% of mixture total weight amount; (ii) the mixture that step (i) is obtained makes the mixture solidified moulding, thereby obtains halogen free flame-proof felt 190-230 ℃ of heating 2-6 minute.
In a preference of the present invention, mix halogen-free flame retardants and bonding agent in the step (i) earlier, with mixed with fibers, obtain mixture then.
In a preference of the present invention, also comprise heating steps in advance, be about to the mixture that step (i) obtains and heated in advance 2-6 minute at 150-180 ℃, obtain first fire retardant felt that solidifies; Described first fire retardant felt that solidifies carries out step and (ii) obtains halogen free flame-proof felt.
The specific embodiment
The inventor is through extensive and deep research, by improving preparation technology, in the mixture of preparation halogen free flame-proof felt, adopt new halogen-free flame retardants, this new halogen-free flame retardants itself just can be used as curing agent bonding agent of the present invention is cured, therefore do not need to add any curing agent, thereby make free ammonia content less than 50ppm, the obtained flame-retardant felt has the excellent fire retardant effect.Thereby halogen-free flame retardants of the present invention further declines to a great extent free ammon amount, so satisfied good flame retardation effect simultaneously, free ammon amount is low, halogen amount is low, minimizing is to the multinomial requirement of the corrosion of metal parts.So be particularly suitable in electrical and electronic component that needs heat-insulating flame-retardant and equipment, using.Finished the present invention on this basis.
The mixture that is used to prepare halogen free flame-proof felt of the present invention comprises following component:
(a) in the fiber of mixture total weight amount 30-80wt%;
(b) in the halogen-free flame retardants of mixture total weight amount 10-60wt%;
(c) in the bonding agent of mixture total weight amount 10-50wt%;
Wherein, described fiber comprises natural fabric, synthetic fiber or its combination;
Described halogen-free flame retardants is salt or its combination that inorganic acid and the metal that is selected from aluminium, calcium, magnesium, zinc form, and wherein said inorganic acid is selected from phosphoric acid, sulfuric acid, boric acid or its combination;
Described bonding agent comprises thermoplastic resin, thermosetting resin or its combination.
Obviously, the halogen free flame-proof felt for preparing of mixture of the present invention is also in protection scope of the present invention.Halogen free flame-proof felt of the present invention can adopt the form of felt, also can adopt the form of the common fire-retardant articles for use in other this area.
Below each technical characterictic of the present invention is described in detail.
Fiber
Fiber of the present invention is selected from one or more of natural fabric, synthetic fiber.Wherein, described natural fabric can be the common natural fabric in this area, for example is selected from cotton, hair, fiber crops or its combination; Described synthetic fiber can be the common synthetic fiber in this area, for example are selected from viscose, polyester fiber, acrylic fibers, polyvinyl chloride fibre, polypropylene fibre or its combination.
Fiber of the present invention can be new, also can select the waste leftover fibrous material for the purpose of saving resource for use and makes through cut-out, refinement, shredding.Among the present invention, the definition of shredding is: the fiber that tangles is opened into monofilament.
Fiber of the present invention accounts for the 30-80wt% of fire retardant felt gross weight, more preferably 40-60wt%.
Halogen-free flame retardants
Described halogen-free flame retardants be inorganic acid be selected from aluminium, calcium, magnesium, zinc, the metal salt or its combination that form, wherein said inorganic acid is selected from phosphoric acid, sulfuric acid, boric acid or its combination.Described salt both can be acid salt, also can be neutral salt.
Preferably, in the described halogen-free flame retardants be the combination of acid salt and neutral salt.Preferably, described acid salt is aluminium dihydrogen phosphate, calcium dihydrogen phosphate or its combination; Described neutral salt is calcium phosphate, magnesium phosphate, aluminum sulfate, wollastonite, Firebrake ZB or its combination.
Preferably, in the gross weight of halogen-free flame retardants, comprise the acid salt of 50-70wt%, the neutral salt of 30-50wt% in the halogen-free flame retardants.
For example, in the example of halogen-free flame retardants of the present invention,, contain the aluminium dihydrogen phosphate of 66wt%, the aluminum sulfate of 17wt%, the Firebrake ZB of 17wt% in the gross weight of halogen-free flame retardants.
The consumption of halogen-free flame retardants accounts for the 10-60wt% of fire retardant felt gross weight, more preferably 20-40wt%.The fire retardant consumption is less than 20wt%, and then flame retardant effect is undesirable; The fire retardant consumption surpasses 40wt%, though the fire retardant felt good flame retardation effect greatly influences the cementability of felt, the contained Dust Capacity of fire retardant felt is increased.
Halogen-free flame retardants of the present invention is preferably pulverous, and its suitable granularity is 2-200 μ m, is preferably 2-100 μ m.
Bonding agent
Optional in thermoplastic resin, thermosetting resin one or more of bonding agent of the present invention also are the mixture that described bonding agent can form for thermoplastic resin, thermosetting resin or thermoplastic resin and thermosetting resin combination.Wherein:
Thermoplastic resin is selected from polyvinyl chloride, polyvinyl acetate, ethylene-vinyl acetate copolymer (EVA), polyamide copolymer as PA6, one or more in PA66 etc., polyethylene and the polypropylene,
Thermosetting resin is selected from one or more in melamino-formaldehyde resin, Lauxite, phenolic resins, epoxy resin, the acetal resin.
Preferably, bonding agent of the present invention adopts the combination of above-mentioned thermoplastic resin and thermosetting resin, the mixture that is combined to form comprises in the thermoplastic resin of bonding agent weight 60-80wt% and the thermosetting resin of 20-40wt%, preferably, contain above-mentioned thermosetting resin in above-mentioned thermoplastic resin of bonding agent weight 65-75wt% and 25-35wt%.
For example, bonding agent comprises in the ethylene-vinyl acetate copolymer of bonding agent gross weight 70wt% with in the Lauxite of bonding agent weight 30wt%.
Or bonding agent comprises in the polyvinyl acetate of bonding agent gross weight 60-80wt% with in the melamino-formaldehyde resin of bonding agent gross weight 20-40wt%.
The consumption of bonding agent accounts for the 10-50wt% of fire retardant felt gross weight, more preferably 20-40wt%.The bonding agent consumption can not be very few, otherwise influence the curing performance of fire retardant felt.
Additive
The mixture of preparation fire retardant felt of the present invention can add the common additive in other this area, as colouring agent, antioxidant.
For example, can in mixture of the present invention, add colouring agent.Past normally by phenolic resins as bonding agent, six methylene tetramines are made curing agent and are come the cured flame-retardant felt, the obtained flame-retardant felted terxture presents the comparatively bright-coloured green of color, so be commonly called as green felt.Constituent of the present invention can for example be allocated colouring agent permanent yellow and bright red (addition is the 0.1-2wt% of fiber) into according to actual needs, and fire retardant felt is dyed various greens.
The preparation method
For realizing the object of the invention, can mix with a certain proportion of fire retardant powder and bonding agent directly with behind the fiber opening, make powder be evenly distributed on the inside and the surface of fiber, be heated to 150～230 ℃ then, preferably, 210～220 ℃ solidify bonding agent, obtain fire retardant felt at last.Sometimes for obtaining the moulding fire retardant felt, also can be at a lower temperature as 120 ℃ of heating the fire retardant felt appearance is solidified, inside also is in the plasticity state, so as under next step operation high temperature further curing molding and obtain required goods.
Fire retardant felt of the present invention does not need to add any curing agent when making, and the obtained flame-retardant felt has excellent fire retardant effect and adhesive property, and free ammonia content is less than 50ppm.
Below in conjunction with specific embodiment, further illustrate the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Ratio and percentage are based on weight, unless stated otherwise.
Embodiment 1
Prepare fire retardant felt by component ratio described in each example of table 1, be specially (wherein the fibrous material chip, the ratio of cotton fiber and polyester fiber is 70/30) pine tag and refinement, get this hairy fiber and add fire retardant powder and the bonding agent that mixes, be heating and curing through 200 ℃ then and just can obtain required fire retardant felt.
Table 1
All components all is unit with the gram in the table 1.
Performance evaluation:
For comparing the performance of fire retardant felt, adopt following method of testing such as UL94 horizontal burning test, free ammonia content, Dust Capacity to be estimated.
UL94 horizontal burning test: carry out the test of horizontal firing foamed material by UL94 " the plastic material inflammability test of equipment and device component " standard.The thickness of test sample batten is 5mm, and flame retardant rating is divided into HBF, HF-1, HF-2 Three Estate.
Free ammonia content test: get about 5 grams of sample that the length of side is not more than 5mm from each position of fire retardant felt material, be soaked in the 100ml pure water and extract, press the Na Shi measuring.
The mensuration of Dust Capacity: with 100cm
2Sample be positioned over that temperature is set is in 150 ℃ the baking oven, take out after 48 hours, freely fall 4 to 5 times, measure because of falling the quality of loss.
The results are shown in Table 2 by above-mentioned method of testing gained.
Table 2
Fire retardant felt of the present invention is mainly used in electronic and electrical equipment, thereby needs the etching problem of metal parts in the consideration equipment.Electronic and electrical equipment for example in the compressor of air conditioner most part be made of copper.If contained free ammonia is higher in the fire retardant felt, will cause copper corrosion.Fire retardant felt free ammonia content of the present invention has satisfied demands of applications less than 50ppm.
The content of halogen is less than 2ppm in described mixture of the present invention or its goods, and the content of free ammonia is less than 50ppm.
All quote in this application as a reference at all documents that the present invention mentions, just quoted as a reference separately as each piece document.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (8)
1. a mixture that is used to prepare halogen free flame-proof felt is characterized in that, described mixture comprises following component:
(a) in the fiber of mixture total weight amount 30-80wt%;
(b) in the halogen-free flame retardants of mixture total weight amount 10-60wt%;
(c) in the bonding agent of mixture total weight amount 10-50wt%;
Wherein, described fiber comprises natural fabric, synthetic fiber or its combination;
Described halogen-free flame retardants is salt or its combination that inorganic acid and the metal that is selected from aluminium, calcium, magnesium, zinc form, and wherein said inorganic acid is selected from phosphoric acid, sulfuric acid, boric acid or its combination;
Described halogen-free flame retardants is selected from the combination of aluminium dihydrogen phosphate, calcium dihydrogen phosphate; Perhaps described halogen-free flame retardants comprises dihydric phosphate in halogen-free flame retardants gross weight 50-70wt%, in the neutral salt of halogen-free flame retardants gross weight 30-50wt%, wherein said dihydric phosphate comprises aluminium dihydrogen phosphate, calcium dihydrogen phosphate or its combination, and described neutral salt comprises calcium phosphate, magnesium phosphate, aluminum sulfate, wollastonite, Firebrake ZB or its combination;
Described bonding agent comprises thermoplastic resin, thermosetting resin or its combination.
2. mixture as claimed in claim 1 is characterized in that, the natural fabric that comprises in the described fiber is selected from cotton, hair, fiber crops or its combination;
Described synthetic fiber are selected from viscose, polyester fiber, acrylic fibers, polyvinyl chloride fibre, polypropylene fibre or its combination.
3. mixture as claimed in claim 1 is characterized in that,
Described thermoplastic resin is selected from polyvinyl chloride, polyvinyl acetate, ethylene-vinyl acetate copolymer, polyamide or its copolymer, polyethylene, polypropylene or its combination;
Described thermosetting resin is selected from melamino-formaldehyde resin, Lauxite, phenolic resins or its combination.
4. mixture as claimed in claim 1 is characterized in that,
Described halogen-free flame retardants comprises in the aluminium dihydrogen phosphate of halogen-free flame retardants gross weight 50-70wt%, in the Firebrake ZB of halogen-free flame retardants gross weight 30-50wt%,
Described bonding agent comprises in the ethylene-vinyl acetate copolymer of bonding agent gross weight 60-80wt%, in the Lauxite of bonding agent gross weight 20-40wt%; Perhaps described bonding agent comprises polyvinyl acetate in bonding agent gross weight 60-80wt%, in the melamino-formaldehyde resin of bonding agent gross weight 20-40wt%.
5. mixture as claimed in claim 1 is characterized in that, described halogen-free flame retardants is the powder of granularity between 2--200 μ m.
6. a method for preparing halogen free flame-proof felt is characterized in that, comprises the steps:
(i) with (a) fiber, (b) halogen-free flame retardants and (c) bonding agent mix, form mixture, wherein said (a) fiber accounts for the 30-80wt% of mixture total weight amount, described (b) halogen-free flame retardants accounts for the 10-60wt% of mixture total weight amount, and described (c) bonding agent accounts for the 10-50wt% of mixture total weight amount;
Described halogen-free flame retardants is selected from the combination of aluminium dihydrogen phosphate, calcium dihydrogen phosphate;
Perhaps described halogen-free flame retardants comprises dihydric phosphate in halogen-free flame retardants gross weight 50-70wt%, in the neutral salt of halogen-free flame retardants gross weight 30-50wt%, wherein said dihydric phosphate comprises aluminium dihydrogen phosphate, calcium dihydrogen phosphate or its combination, and described neutral salt comprises calcium phosphate, magnesium phosphate, aluminum sulfate, wollastonite, Firebrake ZB or its combination;
(ii) the mixture that step (i) is obtained makes the mixture solidified moulding, thereby obtains halogen free flame-proof felt 190-230 ℃ of heating 2-6 minute.
7. method as claimed in claim 6 is characterized in that, mixes halogen-free flame retardants and bonding agent in the step (i) earlier, with mixed with fibers, obtains mixture then.
8. method as claimed in claim 6 is characterized in that, also comprises heating steps in advance, is about to the mixture that step (i) obtains and heats in advance 2-6 minute at 150-180 ℃, obtains first fire retardant felt that solidifies; Described first fire retardant felt that solidifies carries out step and (ii) obtains halogen free flame-proof felt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005101120069A CN1990928B (en) | 2005-12-26 | 2005-12-26 | Halogen free flame-proof felt and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005101120069A CN1990928B (en) | 2005-12-26 | 2005-12-26 | Halogen free flame-proof felt and its preparation method |
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| CN1990928A CN1990928A (en) | 2007-07-04 |
| CN1990928B true CN1990928B (en) | 2010-07-21 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101324025B (en) * | 2008-08-07 | 2010-12-22 | 镇江立达纤维工业有限责任公司 | Non-ammine flame-retardant felt and manufacturing method thereof |
| CN102221528A (en) * | 2011-03-25 | 2011-10-19 | 上海市计量测试技术研究院 | Method for testing concentration of free ammonia in cotton-based baffle blanket |
| CN102277686B (en) * | 2011-07-08 | 2013-04-10 | 镇江立达纤维工业有限责任公司 | Highly flame-retardant felt used for automobile engine compartment and manufacturing method thereof |
| CN102418239A (en) * | 2011-09-13 | 2012-04-18 | 张陆贤 | Method for preparing heat-insulating soundproof damping fibrofelt |
| CN102504390B (en) * | 2011-10-21 | 2014-11-26 | 嵊州市百恩贸易有限公司 | Production method for flame-retardant felt |
| CN102619022B (en) * | 2012-04-24 | 2015-09-09 | 南通大学 | A kind of composite interior material for motor car and preparation method thereof |
| CN103382624A (en) * | 2013-08-13 | 2013-11-06 | 苏州鑫汉纺纺织有限公司 | Novel insulation fabric |
| CN103397475A (en) * | 2013-08-14 | 2013-11-20 | 苏州鑫汉纺纺织有限公司 | Novel fireproof fabric |
| CN105544231A (en) * | 2015-12-23 | 2016-05-04 | 芜湖馨源海绵有限公司 | Felt cushion for automobile trunk and preparation process of felt cushion |
| CN107938353A (en) * | 2017-11-30 | 2018-04-20 | 英泰时尚服饰（苏州）有限公司 | A kind of acrylic fabric and its soft fire-retardant composite finishing method |
| CN110066422A (en) * | 2018-01-20 | 2019-07-30 | 连州市科鑫阻燃技术有限公司 | A kind of white marble phosphorus flame retardant |
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