CN101942763B - Method for manufacturing halogen-free flame retardant nylon sticky buckle strap - Google Patents

Method for manufacturing halogen-free flame retardant nylon sticky buckle strap Download PDF

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CN101942763B
CN101942763B CN2010101850556A CN201010185055A CN101942763B CN 101942763 B CN101942763 B CN 101942763B CN 2010101850556 A CN2010101850556 A CN 2010101850556A CN 201010185055 A CN201010185055 A CN 201010185055A CN 101942763 B CN101942763 B CN 101942763B
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halogen
gluing buckle
chinlon gluing
free flame
retardant
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CN101942763A (en
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郑国烟
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Jiangsu Baihong Composite Material Technology Co ltd
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Wuxi Baihe Weaving Co Ltd
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Abstract

The invention relates to a method for manufacturing a halogen-free flame retardant nylon sticky buckle strap, which comprises the following steps of: cleaning, dyeing, dehydration, sizing finishing, drying, retardant finishing, hot melt adhesive finishing and the like of the nylon sticky buckle strap. In the halogen-free flame retardant nylon sticky buckle strap manufactured by the method, dyes, a sizing finishing agent, a flame retardant finishing agent and a hot melt adhesive finishing agent which used in the production process do not contain halogen or heavy metal, adopt a water-based finishing agent and has zero release and no environmental pollution; compared with the prior art, the halogen-free flame retardant nylon sticky buckle strap improves the flame retardant effect, prevents the burning process from releasing toxic gas, has high visibility and meets the fireproofing safety standard of the American Boeing company and German rail vehicles; and when the halogen-free flame retardant nylon sticky buckle strap is used for sticky buckle straps of vehicles, the safety of persons and the vehicles is improved.

Description

A kind of manufacturing approach of halogen-free flame-retardant chinlon gluing buckle
Technical field
The present invention relates to a kind of manufacturing approach of chinlon gluing buckle, particularly a kind of manufacturing approach of halogen-free flame-retardant chinlon gluing buckle.
Background technology
Halogens comprises fluorine (F), chlorine (Cl), bromine (Br), iodine (I), astatine (At).Wherein astatine (At) is a radioactive element, in product, exists hardly, and fluorine (F), chlorine (Cl), bromine (Br), four kinds of elements of iodine (I) particularly exist with the organic compound form in polymeric material in product.The halogen compounds that is applied at present in the flame retardant products is mainly PBB, PBDE, TBBP-A, PCB, hexabromo dodecane, tribromphenol, short chain chlorinated paraffin wax.
In flame retardant products, add halogen (fluorine, chlorine, bromine, iodine) in order to improve burning-point, its advantage is: burning-point is higher than general polymer material, and burning-point is greatly about 300 ℃.During burning, can give out halogenation gas (fluorine, chlorine, bromine, iodine), absorb oxygen rapidly, thereby fire is extinguished.But its shortcoming is when to be the chlorine gas concentration that discharges high; The visibility decline that causes can cause the survivor can't the escape recognition path, and chlorine has very strong toxicity simultaneously, influences people's respiratory system; In addition; The halogen gas that the halogen containing polymers burning discharges can generate corrosivity pernicious gas (hydrogen halides) when combining with water vapour, some equipment and building are caused corrosion.
PBB, PBDE, brominated flame retardants such as TBBPA use more fire retardant at present, and these halogen containing flame-retardant materials produce dioxin when burning, and in environment, can exist for many years, even accumulate on organism all the life, can't discharge.Therefore, a lot of international major companies abrogate halogen containing material fully actively promoting, as forbid in product, using halogen flame etc.
Existing common flame-proof chinlon gluing buckle all adopts halogen flame; Though have flame retardant effect, when being used for the magic tape of the vehicles such as aircraft, train, automobile, discharge toxic gas easily; Reduce visibility, bring potential safety hazard for the person and the vehicles.
Summary of the invention
For overcoming above defective; The invention provides a kind of manufacturing approach of halogen-free flame-retardant chinlon gluing buckle; Comprise polyamide fibre thread gluing clean-with halogen, heavy metal free dyestuff dye arrangement-dehydration-use, nontoxic, superhard PU resin carry out gluing arrangement-oven dry-with the halogen-free flame-retardant finishing agent put in order-dry-chinlon gluing buckle is carried out step such as PUR arrangement with halogen, heavy metal free PUR, overcome the harm that halogen-containing magic tape brings in the prior art fully with the flame-proof chinlon gluing buckle of the inventive method preparation.The inventive method realizes through following steps:
Step 1: earlier chinlon gluing buckle is put into impregnating mangle and clean, with the finish and the spot of removing fiber surface, during cleaning, the prescription of every processing 180-200 kilogram chinlon gluing buckle cleaning agent is:
Emulsifying agent LF100 900-1000g
Sheet alkali PJ 300-400g
Water 3800-4300Kg
Wherein said emulsifying agent LF100 can be buied by Taiwan hundred grand International Trading Company Ltd, and sheet alkali PJ can be buied by the big negotiation trade of Wuxi City Co., Ltd;
Step 2: the dyestuff that the chinlon gluing buckle after will cleaning puts in the impregnating mangle with halogen, do not contain heavy metal dyes, and the dyeing prescription is:
Dyestuff B lack 2S-LD 2-3%
Emulsifying agent FS-130 0.2-0.6ml/L
Temperature during dyeing is 90-98 ℃, and dyeing time is 2-3 hour, and wherein said dyestuff B lack 2S-LD can knit dyeing technique Co., Ltd and buys by Europe, Shanghai is long-pending, and emulsifying agent FS-130 can be buied by pool, Shanghai star Fine Chemical Co., Ltd;
Step 3: the chinlon gluing buckle dehydration after will dyeing 3-5 minute;
Step 4: the chinlon gluing buckle after will dewatering use, nontoxic, superhard PU resin in gluing machine carry out the gluing arrangement, so that with the locking of chinlon gluing buckle wire gauze, do not decoherence in use, the consumption of PU resin 147 is 100-150g/m during the gluing arrangement 2, described PU polyester 147 can gather prosperous business corporation and buy from Taiwan;
Step 5: the chinlon gluing buckle after the PU resin gluing arrangement was dried 3-5 minute at 100-105 ℃;
Step 6: with isopropyl alcohol as bridging agent; Dilution proportion dissolving fire retardant F200 powder with 1 (isopropyl alcohol weight): 1-1.5 (fire retardant F200 powder weight); Add PU glue PU2835 in the mixture of isopropyl alcohol and fire retardant F200 powder in the ratio of 1 (PU glue PU2835 weight): 9-10 (mixture weight of isopropyl alcohol and fire retardant F200 powder) again; In the agitated reactor of 100 kilograms of capacity, put into 70-80 kilogram PU glue PU2835, isopropyl alcohol and fire retardant F200 powder three's mixture; Logical nitrogen polymerisation is 4-4.5 hour under 65-70 ℃ of condition, stirs 30-40 minute with the titration of 1-1.5 kilogram AD auxiliary agent again, processes antiflaming finishing agent.And in impregnating mangle; At normal temperatures the chinlon gluing buckle of oven dry is carried out dip finishing with the halogen-free flame-retardant finishing agent, make the halogen-free flame-retardant finishing agent be penetrated into chinlon gluing buckle inside, the temperature of dip finishing is 40-60 ℃; Time 1-3 hour; the bath raio ratio of water weight (the magic tape weight with) 1: 10-15, antiflaming finishing agent consumption are the 20-30% of magic tape weight, and fire retardant F200 powder of the present invention and water-based PU glue PU2835 can gather prosperous business corporation from Taiwan; the AD auxiliary agent can be buied from DOW CORNING Shanghai Co., Ltd, and isopropyl alcohol can be buied by medicine chemical plant, Jiangdu;
Step 7: the chinlon gluing buckle that in dryer, will pass through the arrangement of halogen-free flame-retardant finishing agent was 100-105 ℃ of oven dry oven dry 3-5 minute;
Step 8: 70-80 kilogram thermoplastic resin RT-7010 is put in the agitated reactor of 100 kilograms of capacity; Logical nitrogen polymerisation is 2-3 hour under 150-160 ℃ of condition; Add 0.6-0.8 kilogram advection agent SE2200 then, stirred 30-40 minute, preparation halogen, heavy metal free PUR; Described thermoplastic resin RT-7010 can ten Sheng Science and Technology Ltd.s buy from Shanghai, and advection agent SE2200 can buy from organosilicon international trade (Shanghai) Co., Ltd. of SHIN-ETSU HANTOTAI;
Step 9: chinlon gluing buckle is put in order with the PUR that contains halogen-free flame-retardant in gluing machine; Further improve the halogen-free flame-retardant effect on the one hand; Make things convenient for the PUR at the magic tape back side directly to paste on the use thing on the other hand; The wherein said prescription that contains the PUR of fire retardant is: PUR weight: fire retardant F200 powder weight=4-9: 1, and the PUR consumption that contains fire retardant that is used on the chinlon gluing buckle is 220-270g/m 2
Halogen-free flame-retardant chinlon gluing buckle with the inventive method manufacturing has good anti-flaming function; And the injury that has brought to human body when having avoided the halogen burning; It is high to run into combustion case visibility; Meet Boeing Co. and German rail vehicle safety standard, when being used for vehicles magic tape, improved the person and vehicles security.Full water-based finishing agent is adopted in the processing of production process arrangement simultaneously, and zero-emission does not produce environmental pollution.
In the present invention, if not refer in particular to, all percentages are benchmark with the magic tape gross weight all, and all raw materials and equipment all can be buied from market, the conventional method in field under the compound method of each finishing agent all adopts.
The specific embodiment
Specific embodiment given below can further specify the present invention.But they are not to qualification of the present invention.
Embodiment 1: carry out as follows:
1, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles, when chinlon gluing buckle was cleaned, the prescription of 180 kilograms of chinlon gluing buckle cleaning agents of every processing was:
Emulsifying agent LF100 950g
Sheet alkali PJ 350
Water 4000kg
2, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles, chinlon gluing buckle is dyeed, dyeing temperature is 90 ℃, and dyeing time is 2 hours, and the dyeing prescription is:
Dyestuff B lack 2S-LD 2%
Emulsifying agent FS-130 0.2ml/L
With the dehydration of the chinlon gluing buckle after the dyeing 3 minutes.
3, chinlon gluing buckle is put into the JC-CT125-1 gluing machine (can become mechanical Co., Ltd to buy from the village, Xiamen), chinlon gluing buckle is carried out PU resin gluing arrangement, the spread of every square metre of chinlon gluing buckle is:
PU resin 147 100g/m 2
The polyamide fibre thread gluing that the gluing of PU resin was put in order is drying 3 minutes at 100 ℃.
4, with isopropyl alcohol as bridging agent; With 1 (isopropyl alcohol weight): the dilution proportion dissolving fire retardant F200 powder of 1 (fire retardant F200 powder weight); Again in 1 (PU glue PU2835 weight): the ratio of 9 (mixture weight of isopropyl alcohol and fire retardant F200 powder) is added PU glue PU2835 in the mixture of isopropyl alcohol and fire retardant F200 powder; In the agitated reactor of 100 kilograms of capacity, put into 70 kilograms of PU glue PU2835, isopropyl alcohol and fire retardant F200 powder three's mixture; Logical nitrogen polymerisation is 4 hours under 65 ℃ of conditions, stirs 30 minutes with 1 kilogram of AD auxiliary agent titration again, processes antiflaming finishing agent.
5, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles; Using antiflaming finishing agent is 40 ℃ to the temperature that chinlon gluing buckle carries out dip finishing; 1 hour time, the bath raio ratio of water weight (the magic tape weight with) 1: 10, the antiflaming finishing agent consumption is 20% of a magic tape weight.
Chinlon gluing buckle after the antiflaming finishing agent arrangement was dried 3 minutes at 100 ℃.
6,70 kilograms of thermoplastic resin RT-7010 are put in the agitated reactor of 100 kilograms of capacity, logical nitrogen polymerisation is 2 hours under 150 ℃ of conditions, adds 0.6 kilogram of advection agent SE2200 then, stirs then 30 minutes, processes PUR.
7, chinlon gluing buckle is put in the JC-CT125-1 gluing machine, with the PUR arrangement that contains fire retardant, the prescription that contains the PUR of fire retardant is to chinlon gluing buckle:
PUR weight: fire retardant F200 powder weight=4: 1
The PUR consumption that contains fire retardant on every square metre of chinlon gluing buckle is: 220g/m 2
Embodiment 2: carry out as follows:
1, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles, when chinlon gluing buckle was cleaned, the prescription of 190 kilograms of chinlon gluing buckle cleaning agents of every processing was:
Emulsifying agent LF100 900g
Sheet alkali PJ 300g
Water 3800kg
2, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles, chinlon gluing buckle is dyeed, dyeing temperature is 95 ℃, and dyeing time is 2.5 hours, and the dyeing prescription is:
Dyestuff B lack 2S-LD 2.5%
Emulsifying agent FS-130 0.4ml/L
With the dehydration of the chinlon gluing buckle after the dyeing 4 minutes.
3, chinlon gluing buckle is put in the JC-CT125-1 gluing machine, chinlon gluing buckle is carried out PU resin gluing arrangement, the spread of every square metre of chinlon gluing buckle is:
PU resin 147 130g/m 2
The chinlon gluing buckle that the gluing of PU resin was put in order was dried 4 minutes at 102 ℃.
4, with isopropyl alcohol as bridging agent; With 1 (isopropyl alcohol weight): the dilution proportion dissolving fire retardant F200 powder of 1.3 (fire retardant F200 powder weight); Again in 1 (PU glue PU2835 weight): the ratio of 9.5 (mixture weight of isopropyl alcohol and fire retardant F200 powder) is added PU glue PU2835 in the mixture of isopropyl alcohol and fire retardant F200 powder; In the agitated reactor of 100 kilograms of capacity, put into 75 kilograms of water-based PU glue PU2835, isopropyl alcohol and fire retardant F200 powder threes' mixture; Logical nitrogen polymerisation is 4.2 hours under 68 ℃ of conditions, stirs 35 minutes with 1.3 kilograms of AD auxiliary agent titration again, processes antiflaming finishing agent.
5, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles; Using antiflaming finishing agent is 50 ℃ to the temperature that chinlon gluing buckle carries out dip finishing; 2 hours time, the bath raio ratio of water weight (the magic tape weight with) 1: 13, the antiflaming finishing agent consumption is 25% of a magic tape weight.
Chinlon gluing buckle after the antiflaming finishing agent arrangement was dried 4 minutes at 102 ℃.
6,75 kilograms of thermoplastic resin RT-7010 are put in the agitated reactor of 100 kilograms of capacity, logical nitrogen polymerisation is 2.5 hours under 155 ℃ of conditions, adds 0.7 kilogram of advection agent SE2200 then, stirs then 35 minutes, processes PUR.
7, chinlon gluing buckle is put in the JC-CT125-1 gluing machine, with the PUR arrangement that contains fire retardant, the prescription that contains the PUR of fire retardant is to chinlon gluing buckle:
PUR weight: fire retardant F200 powder weight=7: 1
The PUR consumption that contains fire retardant on every square metre of chinlon gluing buckle is: 250g/m 2
Embodiment 3: carry out as follows:
1, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles, when chinlon gluing buckle was cleaned, the prescription of 200 kilograms of chinlon gluing buckle cleaning agents of every processing was:
Emulsifying agent LF100 1000g
Sheet alkali PJ 400g
Water 4300Kg
2, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles, chinlon gluing buckle is dyeed, dyeing temperature is 98 ℃, and dyeing time is 3 hours, and the dyeing prescription is:
Dyestuff Black 2S-LD 3%
Emulsifying agent FS-130 0.6ml/L
With the dehydration of the chinlon gluing buckle after the dyeing 5 minutes.
3, chinlon gluing buckle is put into the JC-CT125-1 gluing machine (can become mechanical Co., Ltd to buy from the village, Xiamen), chinlon gluing buckle is carried out PU resin gluing arrangement, the spread of every square metre of chinlon gluing buckle is:
PU resin 147 150g/m 2
The chinlon gluing buckle that the gluing of PU resin was put in order was dried 5 minutes at 105 ℃.
4, with isopropyl alcohol as bridging agent; With 1 (isopropyl alcohol weight): the dilution proportion dissolving fire retardant F200 powder of 1.5 (fire retardant F200 powder weight); Again in 1 (PU glue PU2835 weight): the ratio of 10 (mixture weight of isopropyl alcohol and fire retardant F200 powder) is added PU glue PU2835 in the mixture of isopropyl alcohol and fire retardant F200 powder; In the agitated reactor of 100 kilograms of capacity, put into 80 kilograms of PU glue PU2835, isopropyl alcohol and fire retardant F200 powder three's mixture; Logical nitrogen polymerisation is 4.5 hours under 70 ℃ of conditions, stirs 40 minutes with 1.5 kilograms of AD auxiliary agent titration again, processes antiflaming finishing agent.
5, chinlon gluing buckle is put in four jiaos of cylinder impregnating mangles; Using antiflaming finishing agent is 60 ℃ to the temperature that chinlon gluing buckle carries out dip finishing; 3 hours time, the bath raio ratio of water weight (the magic tape weight with) 1: 15, the antiflaming finishing agent consumption is 30% of a magic tape weight.
Chinlon gluing buckle after the antiflaming finishing agent arrangement was dried 5 minutes at 105 ℃.
6,80 kilograms of thermoplastic resin RT-7010 are put in the agitated reactor of 100 kilograms of capacity, logical nitrogen polymerisation is 3 hours under 160 ℃ of conditions, adds 0.8 kilogram of advection agent SE2200 then, stirs then 40 minutes, processes PUR.
7, chinlon gluing buckle is put in the JC-CT125-1 gluing machine, with the PUR arrangement that contains fire retardant, the prescription that contains the PUR of fire retardant is to chinlon gluing buckle:
PUR weight: fire retardant F200 powder weight=9: 1
The PUR consumption that contains fire retardant on every square metre of chinlon gluing buckle is: 270g/m 2
Meet at flame retardant effect under the condition of the technical specification BSS7238:1997 of Boeing Co.; The experimental result of halogen-free flame-retardant chinlon gluing buckle of the present invention and existing common flame-proof chinlon gluing buckle contrast (according to test of U.S. Boeing technical specification BSS7238:1997 material combustion method of testing and evaluation optical density, according to German rail vehicle fire-protection standard DIN5510-2:2009Annex C test and evaluation of flue gas toxicity) as shown in table 1:
Table 1
Figure GSA00000122487500071
Visible from table 1, sample light density of the present invention (characterizing the index of visibility) and flue gas toxity index are lower than common flame-proof chinlon gluing buckle, meet standard fully.

Claims (7)

1. the manufacturing approach of a halogen-free flame-retardant chinlon gluing buckle; Comprise to polyamide fibre that thread gluing is cleaned, dyeed, dehydration, gluing arrangement, baking step; When it is characterized in that chinlon gluing buckle cleaned, the prescription of every processing 180-200 kilogram chinlon gluing buckle cleaning agent is:
Emulsifying agent LF100 900-1000g
Sheet alkali PJ 300-400g
Water 3800-4300kg;
Chinlon gluing buckle to after the oven dry carries out flame-proof treatment; Oven dry again; Prepare halogen, heavy metal free PUR afterwards, and chinlon gluing buckle is carried out the PUR arrangement, wherein said fire retarding treating liquid is as bridging agent with isopropyl alcohol; Isopropyl alcohol and fire retardant F200 powder are with 1: the mixed of 1-1.5; Again PU glue and said mixture are pressed 1: the mixed of 9-10, logical nitrogen polymerisation is 4-4.5 hour under 65-70 ℃ of condition, stirs with the titration of 1-1.5 kilogram AD auxiliary agent afterwards and processes in 30-40 minute; Described PUR is that 70-80 kilogram thermoplastic resin RT-7010 is put in the agitated reactor, and logical nitrogen polymerisation is 2-3 hour under 150-160 ℃ of condition, adds 0.6-0.8 kilogram advection agent SE2200 then, stirs and processes in 30-40 minute; When chinlon gluing buckle is put in order with the PUR that contains halogen-free flame-retardant, described PUR weight: fire retardant F200 powder weight=4-9: 1.
2. the manufacturing approach of halogen-free flame-retardant chinlon gluing buckle as claimed in claim 1; It is characterized in that the temperature of using antiflaming finishing agent to carry out dip finishing is 40-60 ℃; Time is 1-3 hour; The ratio 1 of magic tape weight and water weight: 10-15, the antiflaming finishing agent consumption is the 20-30% of magic tape weight, the chinlon gluing buckle after flame-proof treatment was 100-105 ℃ of oven dry 3-5 minute.
3. according to claim 1 or claim 2 the manufacturing approach of halogen-free flame-retardant chinlon gluing buckle; It is characterized in that isopropyl alcohol and fire retardant F200 powder are with 1: the mixed of 1-1.3; Again with PU glue and said mixture mixed by 1: 9.5; Logical nitrogen polymerisation is 4.2 hours under 68 ℃ of conditions, stirs with 1.3 kilograms of AD auxiliary agent titration afterwards and processes in 35 minutes; Described PUR is that 75 kilograms of thermoplastic resin RT-7010 are put in the agitated reactor, and logical nitrogen polymerisation is 2.5 hours under 155 ℃ of conditions, adds 0.7 kilogram of advection agent SE2200 then, stirs and processes in 35 minutes.
4. according to claim 1 or claim 2 the manufacturing approach of halogen-free flame-retardant chinlon gluing buckle, its characteristic
Be that the dyeing prescription is:
Dyestuff B1ack 2S-LD 2-3%
Emulsifying agent FS-130 0.2-0.6ml/L.
5. according to claim 1 or claim 2 the manufacturing approach of halogen-free flame-retardant chinlon gluing buckle is characterized in that dyeing temperature is 90-98 ℃, and dyeing time is 2-3 hour, and the dewatering time of dyeing back chinlon gluing buckle is 3-5 minute.
6. according to claim 1 or claim 2 the manufacturing approach of halogen-free flame-retardant chinlon gluing buckle, PU resin 147 is 100-150g/m when it is characterized in that the gluing arrangement 2, after the gluing arrangement chinlon gluing buckle was dried 3-5 minute at 100-105 ℃.
7. according to claim 1 or claim 2 the manufacturing approach of halogen-free flame-retardant chinlon gluing buckle is characterized in that the PUR consumption that contains fire retardant on the chinlon gluing buckle is: 220-270g/m 2
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