CN106868883A - A kind of preparation method of aqueous figured type flame-proof environmental protection suede - Google Patents

A kind of preparation method of aqueous figured type flame-proof environmental protection suede Download PDF

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Publication number
CN106868883A
CN106868883A CN201710022810.0A CN201710022810A CN106868883A CN 106868883 A CN106868883 A CN 106868883A CN 201710022810 A CN201710022810 A CN 201710022810A CN 106868883 A CN106868883 A CN 106868883A
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aqueous
area
drying
parts
figured type
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CN106868883B (en
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孙进琳
王友忠
李银林
姜沈富
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Zhejiang Fansheng Microfiber Products Co Ltd
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Zhejiang Fansheng Microfiber Products Co Ltd
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
    • D06N3/145—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes two or more layers of polyurethanes
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Abstract

The present invention relates to leather sector, a kind of preparation method of aqueous figured type flame-proof environmental protection suede is disclosed, comprised the following steps：1）Pre- impregnation；2）Drying；3）Scald contracting；4）Main impregnation；5）Drying；6）Alkali reduction；7）Drying stoking；8）Buffing；9）Dyeing；10）Drying and shaping, final finished product.Suede obtained in the inventive method uses aqueous materials, environmental protection；And its anti-flammability, mechanical performance, hygroscopicity, gas permeability, antibacterial anti-mildew are outstanding.

Description

A kind of preparation method of aqueous figured type flame-proof environmental protection suede
Technical field
The present invention relates to leather sector, more particularly to a kind of preparation method of aqueous figured type flame-proof environmental protection suede.
Background technology
At present, the most synthetic leather of in the market uses solvent borne polyurethane, and the solvent borne polyurethane feature of environmental protection is poor, is producing Organic solvent volatile quantity is big in journey, does not meet the trend of current environmental protection.Because aqueous polyurethane is with water as decentralized medium, There is no the volatilization of solvent in production process, it is environmentally safe, to the operating personnel of workshop without health hazard, more environmental protection It is harmless.Meanwhile, there is no peculiar smell in aqueous polyurethane production process, nonflammable, process is safe and reliable.As people live The continuous improvement of quality, aqueous polyurethane is more and more applied in synthetic leather field.
As Application No. CN201110232140.8 Chinese patent disclose a kind of Micro-fiber environment-friendlywater-base water-base synthetic leather and its Preparation method, the synthetic leather includes woven fabric non-woven fabrics, the bottom being covered on non-woven fabrics, and is covered in the surface layer on bottom, Wherein, surface layer includes that at least 4 layers are scraped the coating for being formed by slurry painting, and each slurry includes：Aqueous polyurethane, water and aqueous Auxiliary agent.The synthetic leather is by using waterborne polyurethane resin, it is to avoid use solvent type polyurethane resin so that prepared conjunction Finished leather environmental protection, does not harm human body..
Although above-mentioned synthetic leather employs aqueous polyurethane, in the market for for waterborne polyurethane synthetic leather Aqueous fire retardant it is still deficient, be always leather industry in the urgent need to address.Additionally, existing synthetic leather is in antibacterial anti-mildew The aspect such as property, pliability, wearability, hygroscopicity and gas permeability is remained to be further improved.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of preparation side of aqueous figured type flame-proof environmental protection suede Method.Suede obtained in the inventive method uses aqueous materials, environmental protection；And its anti-flammability, mechanical performance, hygroscopicity, thoroughly Gas, antibacterial anti-mildew are outstanding.
Concrete technical scheme of the invention is：A kind of preparation method of aqueous figured type flame-proof environmental protection suede, including with Lower step：
1) pre- impregnation：By figured type superfine fibre nonwoven cloth in modified wool fat liquor impregnation process, then take out non-woven fabrics And wipe unnecessary emulsion away, then by non-woven fabrics it is aqueous it is pre- containing immersion liquid in carry out pre- impregnation；It is described it is aqueous it is pre- containing immersion liquid by following Parts by weight of component is constituted：35-45 parts of waterborne polyurethane resin, 155-165 parts of water.
2) dry：Non-woven fabrics after pre- impregnation is dried.
3) contracting is scalded：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting.
4) main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, the ultra-fine fibre of figured type is obtained Dimension bass；Aqueous master includes the component of following weight portion containing immersion liquid：0.05-0.15 parts of aqueous color, 35-45 parts of water, 25-35 parts Waterborne polyurethane resin, 3-5 parts of nanometer galapectite pipe, 1-2 parts of aqueous dispersion, 6-8 parts of halogen-free type fireproof powder, 6-8 parts of PA without Halogen environmental protection fire retarding agent, 0.1-0.3 parts of defoamer.
5) dry：Figured type superfine fibre bass to being obtained after main impregnation is dried.
6) Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed.In Alkali reduction During sea component dissolving in figured type superfine fibre, be left island component.
7) stoking is dried：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long.
8) buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking.
9) dye.
10) drying and shaping, final finished product.
The present invention with figured type superfine fibre nonwoven cloth as base fabric, from aqueous polyurethane, aqueous color, aqueous fire retardant It is impregnated with Deng raw material.Whole preparation technology is more environmentally friendly, low toxicity evil.Especially coordinate PA Halogen rings from halogen-free type fireproof powder Used as fire retardant, with aqueous polyurethane compatibility, obtained suede flame retardant effect is more preferably for environment friendly flame-retardant agent.
In preparation process, the present invention originally first uses modified wool fat liquor degree non-woven fabrics impregnation process, and be modified sheep Hair fat be oily matter, good film-forming property, fiber surface is wrapped by after treatment, formed a tunic.Benefit is in follow-up impregnation process Middle fiber can avoid directly being bonded with polyurethane and causing non-woven fabrics to harden, not submissive enough.In addition lanolin can also be improved The hygroscopicity of non-woven fabrics.
The present invention carries out pre- impregnation-drying-scald and contract before main impregnation, can make to be penetrated sufficiently between fiber containing immersion liquid Space, improve non-woven fabrics to the absorptivity containing immersion liquid, so as to improve the intensity of product.And first pre- impregnation-scald contracting, then master contains Leaching, compared with contracting is scalded after direct main impregnation；Because polyurethane and non-woven fabrics occur pyrocondensation when the latter scalds contracting, leather surface can be caused to go out Existing fold and it is not smooth enough, and internal stress cannot eliminate.And the technique for being impregnated with-scalding contracting-main impregnation in advance can then overcome this skill Art problem.The present invention is also originally added with a nanometer galapectite pipe in aqueous master contains immersion liquid, and nanometer galapectite pipe is nanometer The tubular inorganic material with hollow hole of rank, with preferable adsorptivity, after solidifying to form leather surface with polyurethane compounding, energy Enough play a part of moisture absorption, improve the hygroscopicity and gas permeability of product.The wearability that it can also improve synthetic leather simultaneously.
Preferably, the figured type superfine fibre nonwoven cloth is obtained by determining island sea-island composite fiber, it is described to determine island sea Island component is PA6 in island superfine fibre, and sea component is COPET；Island number is 30-180, and determining island sea-island composite fiber fiber number is 0.5-5dtex, non-woven fabrics grammes per square metre is in 150-500g/cm2, density 0.16-0.22g/cm2。
The present invention selects above-mentioned specific figured type superfine fibre nonwoven cloth, and its intensity is high, and the suede after-drawing of system is light Degree, tearing toughness are outstanding.After the dissolving of its sea component, island component compliance is good, it is possible to increase the feel of suede.
Preferably, the modified wool fat liquor is made up of following parts by weight of component：25-35 parts of modified wool fat, 55- 75 parts of water and 4-6 parts of emulsifying agent composition；The preparation method of the modified wool fat is as follows：Lanolin is heated in liquid, Then the phosphorus pentoxide of its quality 6-8% is at the uniform velocity added during used time 40-50min is to lanolin under the heat-retaining condition；Reaction knot Shu Hou, it is neutral to adjust liquid with alkali lye, and modified wool fat is obtained after drying.
Natural wool fat is harder, and mobility is poor, and film forming is poor, poorly water-soluble, is difficult emulsification, is unfavorable in fiber surface Film forming.Present invention demand of the invention, is modified to lanolin, with the modified softening of phosphorus pentoxide, mobility, into Film strengthens, and is more easy to emulsification.And modified generation bound phosphate groups, with certain antibacterial and mouldproof, so as to assign matte Leather antibacterial and antimildew function, kills two birds with one stone.
Preferably, step 2) drying temperature setting it is as follows：First 85-95 DEG C of area, the second 100-110 DEG C of area, the 3rd 110-120 DEG C of area, the 4th 120-130 DEG C of area, the 5th 130-135 DEG C of area, drying rate：5-6 meters/min.
Preferably, step 3) boiling hot compression roller gap be 0.8-1.4mm, temperature be 110-130 DEG C, speed be 5-6 meters/ min。
Preferably, the nanometer galapectite pipe is processed by ion modification, method is as follows：By the dispersion of nanometer galapectite pipe It is the suspension of 10-20% that Yu Shuizhong forms mass concentration；Nitrate solution containing magnesium ion and iron ion is added drop-wise to not In the suspension of disconnected stirring, the nanometer galapectite pipe for being loaded with metal ion, wherein magnesium ion are centrifugally separating to obtain after dripping It is 1-2mol/L with the concentration of iron ion, the dripping quantity of nitrate is the 20-40% of suspension quality；Used again silane coupled Agent is modified, and ion modification nanometer galapectite pipe is obtained after drying.
To nanometer galapectite pipe modification, nanometer galapectite pipe surface has hydroxyl to the present invention, with ion exchange, inhales Attached ability, is loaded with metal ion on modified nanometer galapectite pipe, the metal ion of the different prices energy under certain humidity Potential difference is enough formed, micro- magnetic field is formed, metal ion can improve the antibacterial activity of itself in the presence of micro- magnetic field, so that Obtaining suede being capable of antibacterial and mouldproof.Nanometer galapectite pipe can play damping, ventilative, wear-resisting work in the present invention as from the foregoing With, again can be used as the carrier of metal ion, performance antibacterial and mouldproof effect.Therefore need not separately be added in suede has to human body Evil, the antibacterial mildew inhibitor of bad dispersibility.
Preferably, step 5) drying temperature setting it is as follows：First 85-95 DEG C of area, the second 100-110 DEG C of area, the 3rd 110-120 DEG C of area, the 4th 120-130 DEG C of area, the 5th 130-135 DEG C of area, the 6th 135-140 DEG C of area；Drying rate be 5-6 meters/ min。
Preferably, step 6) Alkali reduction when, alkali concn is 7-10%, and steam box temperature is 90-95 DEG C, and speed is 5-6 Rice/min, washing water-carrying capacity is 1-2 tons/h.
Preferably, step 7) in, stoking goes out to remove from office speed 5-6 meters/min, and temperature is set as：First 95-100 DEG C of area, the Two 120-125 DEG C of areas, the 3rd 120-125 DEG C of area, the 4th 125-135 DEG C of area, the 5th 130-135 DEG C of area.
Preferably, step 8) in, buffing interval gap is set as：First interval gap 0.6-1.6mm, abrasive band 180-320 mesh, Second interval gap 0.4-1.4mm, abrasive band 320-600 mesh, speed 5-6 meters/min.
The setting of above-mentioned each process parameter, is the present inventor's non-woven fabrics base fabric of the invention, various impregnations Liquid and specific setting.Cooperated before and after the technological parameter of above-mentioned each step under association, cooperation, this hair can be obtained The excellent suede of bright various aspects of performance.Its each step is not that the simple of ordinary skill in the art means is pieced together.
It is compared with the prior art, the beneficial effects of the invention are as follows：Suede uses aqueous materials obtained in the inventive method, Environmental protection；And its anti-flammability, mechanical performance, hygroscopicity, gas permeability, antibacterial anti-mildew are outstanding.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of aqueous figured type flame-proof environmental protection suede, comprises the following steps：
1) pre- impregnation：From figured type superfine fibre nonwoven cloth as raw material, the non-woven fabrics is by determining island sea-island composite fiber system , described determine island component in the sea-island composite fiber of island be PA6, and sea component is COPET；Island number is 37, determines island fabric of island-in-sea type ultra-fine Fibre number is 2.64dtex, and non-woven fabrics grammes per square metre is in 320g/cm2, density 0.19g/cm2.Figured type superfine fibre nonwoven cloth is existed Impregnation process 30min in modified wool fat liquor, then takes out non-woven fabrics and wipes unnecessary emulsion away, then by non-woven fabrics aqueous In advance containing carrying out pre- impregnation in immersion liquid.
Wherein, the modified wool fat liquor is made up of following parts by weight of component：30 parts of modified wool fat, 65 parts of water and 5 Part emulsifying agent composition；The preparation method of the modified wool fat is as follows：Lanolin is heated in liquid, then in heat preservation strip Part lower used time 45min is to the phosphorus pentoxide that its quality 7% is at the uniform velocity added in lanolin；After reaction terminates, liquid is adjusted with alkali lye Body is neutrality, and modified wool fat is obtained after drying.
It is described aqueous pre- to be made up of following parts by weight of component containing immersion liquid：40 parts of waterborne polyurethane resin AE-12,160 parts of water.
2) dry：Non-woven fabrics after pre- impregnation is dried.Drying temperature setting is as follows：First 90 DEG C of area, the secondth area 105 DEG C, the 3rd 115 DEG C of area, the 4th 125 DEG C of area, the 5th 132 DEG C of area, drying rate：5.5 meters/min.
3) contracting is scalded：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting.It is 1.1mm to scald compression roller gap, and temperature is 120 DEG C, speed is 5.5 meters/min.
4) main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, the ultra-fine fibre of figured type is obtained Dimension bass；Aqueous master includes the component of following weight portion containing immersion liquid：0.10 part of aqueous color, 40 parts of water, 30 parts of aqueous polyurethanes Resin A E-12,4 parts of nanometer galapectite pipes, 1.5 parts of aqueous dispersion AR-312,7 parts of halogen-free type fireproof powder Exolit op935,7 Part PA halogen-free environment-friendlyflame flame retardant Exolit op1240,0.2 part of defoamer.
The nanometer galapectite pipe is processed by ion modification, and method is as follows：Nanometer galapectite pipe is dispersed in water shape Into the suspension that mass concentration is 15%；Nitrate solution containing magnesium ion and iron ion is added drop-wise to be stirred continuously suspended In liquid, the nanometer galapectite pipe for being loaded with metal ion is centrifugally separating to obtain after dripping, wherein magnesium ion and iron ion is dense It is 1.5mol/L to spend, and the dripping quantity of nitrate is the 30% of suspension quality；Used silane coupler modified again, after drying To ion modification nanometer galapectite pipe.
5) dry：Figured type superfine fibre bass to being obtained after main impregnation is dried.Drying temperature setting is as follows：The One 90 DEG C of area, the second 105 DEG C of area, the 3rd 115 DEG C of area, the 4th 125 DEG C of area, the 5th 132 DEG C of area, the 6th 138 DEG C of area；Drying rate It is 5.5 meters/min.
6) Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed.Alkali reduction When, alkali concn is 8.5%, and steam box temperature is 93 DEG C, and speed is 5.5 meters/min, and washing water-carrying capacity is 1.5 tons/h.
7) stoking is dried：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long.Stoking goes out leather speed 5.5 meters/min of degree, temperature is set as：First 98 DEG C of area, the second 122 DEG C of area, the 3rd 124 DEG C of area, the 4th 130 DEG C of area, the 5th area 133℃。
8) buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking.Buffing interval gap is set as：First Interval gap 1.1mm, the mesh of abrasive band 250, second interval gap 0.9mm, the mesh of abrasive band 460,5.5 meters/min of speed.
9) dye.
10) drying and shaping, final finished product.
Embodiment 2
A kind of preparation method of aqueous figured type flame-proof environmental protection suede, comprises the following steps：
1) pre- impregnation：From figured type superfine fibre nonwoven cloth as raw material, the non-woven fabrics is by determining island sea-island composite fiber system , described determine island component in the sea-island composite fiber of island be PA6, and sea component is COPET；Island number is 180, determines island fabric of island-in-sea type ultra-fine Fibre number is 2.57dtex, and non-woven fabrics grammes per square metre is in 150g/cm2, density 0.16g/cm2.Figured type superfine fibre nonwoven cloth is existed Impregnation process 20min in modified wool fat liquor, then takes out non-woven fabrics and wipes unnecessary emulsion away, then by non-woven fabrics aqueous In advance containing carrying out pre- impregnation in immersion liquid.
Wherein, the modified wool fat liquor is made up of following parts by weight of component：25 parts of modified wool fat, 71 parts of water and 4 Part emulsifying agent composition；The preparation method of the modified wool fat is as follows：Lanolin is heated in liquid, then in heat preservation strip Part lower used time 40min is to the phosphorus pentoxide that its quality 6% is at the uniform velocity added in lanolin；After reaction terminates, liquid is adjusted with alkali lye Body is neutrality, and modified wool fat is obtained after drying.
It is described aqueous pre- to be made up of following parts by weight of component containing immersion liquid：35 parts of waterborne polyurethane resin AE-12,155 parts of water.
2) dry：Non-woven fabrics after pre- impregnation is dried.Drying temperature setting is as follows：First 85 DEG C of area, the secondth area 100 DEG C, the 3rd 110 DEG C of area, the 4th 120 DEG C of area, the 5th 130 DEG C of area, drying rate：5 meters/min.
3) contracting is scalded：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting.It is 0.8mm to scald compression roller gap, and temperature is 110 DEG C, speed is 5 meters/min.
4) main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, the ultra-fine fibre of figured type is obtained Dimension bass；Aqueous master includes the component of following weight portion containing immersion liquid：0.05 part of aqueous color, 35 parts of water, 25 parts of aqueous polyurethanes Resin A E-12,3 parts of nanometer galapectite pipes, 1 part of aqueous dispersion AR-312,6 parts of halogen-free type fireproof powder Exolit op935,6 parts PA halogen-free environment-friendlyflame flame retardant Exolit op1240,0.1 part of defoamer.
The nanometer galapectite pipe is processed by ion modification, and method is as follows：Nanometer galapectite pipe is dispersed in water shape Into the suspension that mass concentration is 10%；Nitrate solution containing magnesium ion and iron ion is added drop-wise to be stirred continuously suspended In liquid, the nanometer galapectite pipe for being loaded with metal ion is centrifugally separating to obtain after dripping, wherein magnesium ion and iron ion is dense It is 1mol/L to spend, and the dripping quantity of nitrate is the 20% of suspension quality；Used silane coupler modified again, obtained after drying Ion modification nanometer galapectite pipe.
5) dry：Figured type superfine fibre bass to being obtained after main impregnation is dried.Drying temperature setting is as follows：The One 85 DEG C of area, the second 100 DEG C of area, the 3rd 110 DEG C of area, the 4th 120 DEG C of area, the 5th 130 DEG C of area, the 6th 135 DEG C of area；Drying rate It is 5 meters/min.
6) Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed.Alkali reduction When, alkali concn is 7%, and steam box temperature is 90 DEG C, and speed is 5 meters/min, and washing water-carrying capacity is 1 ton/h.
7) stoking is dried：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long.Stoking goes out leather speed 5 meters/min of degree, temperature is set as：First 95 DEG C of area, the second 120 DEG C of area, the 3rd 120 DEG C of area, the 4th 125 DEG C of area, the 5th area 130 ℃。
8) buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking.Buffing interval gap is set as：First Interval gap 0.6mm, the mesh of abrasive band 180, second interval gap 0.4mm, the mesh of abrasive band 320,5 meters/min of speed.
9) dye.
10) drying and shaping, final finished product.
Embodiment 3
A kind of preparation method of aqueous figured type flame-proof environmental protection suede, comprises the following steps：
1) pre- impregnation：From figured type superfine fibre nonwoven cloth as raw material, the non-woven fabrics is by determining island sea-island composite fiber system , described determine island component in the sea-island composite fiber of island be PA6, and sea component is COPET；Island number is 44, determines island fabric of island-in-sea type ultra-fine Fibre number is 5dtex, and non-woven fabrics grammes per square metre is in 500g/cm2, density 0.22g/cm2.Figured type superfine fibre nonwoven cloth is being changed Impregnation process 40min in property wool fat liquor, then takes out non-woven fabrics and wipes unnecessary emulsion away, then by non-woven fabrics aqueous pre- Containing carrying out pre- impregnation in immersion liquid.
Wherein, the modified wool fat liquor is made up of following parts by weight of component：35 parts of modified wool fat, 59 parts of water and 6 Part emulsifying agent composition；The preparation method of the modified wool fat is as follows：Lanolin is heated in liquid, then in heat preservation strip Part lower used time 50min is to the phosphorus pentoxide that its quality 8% is at the uniform velocity added in lanolin；After reaction terminates, liquid is adjusted with alkali lye Body is neutrality, and modified wool fat is obtained after drying.
It is described aqueous pre- to be made up of following parts by weight of component containing immersion liquid：45 parts of waterborne polyurethane resin AE-12,165 parts of water.
2) dry：Non-woven fabrics after pre- impregnation is dried.Drying temperature setting is as follows：First 95 DEG C of area, the secondth area 110 DEG C, the 3rd 120 DEG C of area, the 4th 130 DEG C of area, the 5th 135 DEG C of area, drying rate：6 meters/min.
3) contracting is scalded：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting.It is 1.4mm to scald compression roller gap, and temperature is 130 DEG C, speed is 6 meters/min.
4) main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, the ultra-fine fibre of figured type is obtained Dimension bass；Aqueous master includes the component of following weight portion containing immersion liquid：0.15 part of aqueous color, 45 parts of water, 35 parts of aqueous polyurethanes Resin A E-12,5 parts of nanometer galapectite pipes, 2 parts of aqueous dispersion AR-312,8 parts of halogen-free type fireproof powder Exolit op935,8 parts PA halogen-free environment-friendlyflame flame retardant Exolit op1240,0.3 part of defoamer.
The nanometer galapectite pipe is processed by ion modification, and method is as follows：Nanometer galapectite pipe is dispersed in water shape Into the suspension that mass concentration is 20%；Nitrate solution containing magnesium ion and iron ion is added drop-wise to be stirred continuously suspended In liquid, the nanometer galapectite pipe for being loaded with metal ion is centrifugally separating to obtain after dripping, wherein magnesium ion and iron ion is dense It is 2mol/L to spend, and the dripping quantity of nitrate is the 40% of suspension quality；Used silane coupler modified again, obtained after drying Ion modification nanometer galapectite pipe.
5) dry：Figured type superfine fibre bass to being obtained after main impregnation is dried.Drying temperature setting is as follows：The One 95 DEG C of area, the second 110 DEG C of area, the 3rd 120 DEG C of area, the 4th 130 DEG C of area, the 5th 135 DEG C of area, the 6th 140 DEG C of area；Drying rate It is 6 meters/min.
6) Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed.Alkali reduction When, alkali concn is 10%, and steam box temperature is 95 DEG C, and speed is 6 meters/min, and washing water-carrying capacity is 2 tons/h.
7) stoking is dried：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long.Stoking goes out leather speed 6 meters/min of degree, temperature is set as：First 100 DEG C of area, the second 125 DEG C of area, the 3rd 125 DEG C of area, the 4th 135 DEG C of area, the 5th area 135℃。
8) buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking.Buffing interval gap is set as：First Interval gap 1.6mm, the mesh of abrasive band 320, second interval gap 1.4mm, the mesh of abrasive band 600,6 meters/min of speed.
9) dye.
10) drying and shaping, final finished product.
Embodiment 4
A kind of preparation method of aqueous figured type flame-proof environmental protection suede, comprises the following steps：
1) pre- impregnation：From figured type superfine fibre nonwoven cloth as raw material, the non-woven fabrics is by determining island sea-island composite fiber system , described determine island component in the sea-island composite fiber of island be PA6, and sea component is COPET；Island number is 30, determines island fabric of island-in-sea type ultra-fine Fibre number is 0.5dtex, and non-woven fabrics grammes per square metre is in 400g/cm2, density 0.19g/cm2.Figured type superfine fibre nonwoven cloth is existed Impregnation process 25min in modified wool fat liquor, then takes out non-woven fabrics and wipes unnecessary emulsion away, then by non-woven fabrics aqueous In advance containing carrying out pre- impregnation in immersion liquid.
Wherein, the modified wool fat liquor is made up of following parts by weight of component：30 parts of modified wool fat, 65 parts of water and 5 Part emulsifying agent composition；The preparation method of the modified wool fat is as follows：Lanolin is heated in liquid, then in heat preservation strip Part lower used time 45min is to the phosphorus pentoxide that its quality 7% is at the uniform velocity added in lanolin；After reaction terminates, liquid is adjusted with alkali lye Body is neutrality, and modified wool fat is obtained after drying.
It is described aqueous pre- to be made up of following parts by weight of component containing immersion liquid：35 parts of waterborne polyurethane resin AE-12,165 parts of water.
2) dry：Non-woven fabrics after pre- impregnation is dried.Drying temperature setting is as follows：First 85 DEG C of area, the secondth area 105 DEG C, the 3rd 115 DEG C of area, the 4th 125 DEG C of area, the 5th 130 DEG C of area, drying rate：5 meters/min.
3) contracting is scalded：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting.It is 1.0mm to scald compression roller gap, and temperature is 115 DEG C, speed is 5 meters/min.
4) main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, the ultra-fine fibre of figured type is obtained Dimension bass；Aqueous master includes the component of following weight portion containing immersion liquid：0.10 part of aqueous color, 40 parts of water, 30 parts of aqueous polyurethanes Resin A E-12,3 parts of nanometer galapectite pipes, 2 parts of aqueous dispersion AR-312,7 parts of halogen-free type fireproof powder Exolit op935,6 parts PA halogen-free environment-friendlyflame flame retardant Exolit op1240,0.2 part of defoamer.
The nanometer galapectite pipe is processed by ion modification, and method is as follows：Nanometer galapectite pipe is dispersed in water shape Into the suspension that mass concentration is 15%；Nitrate solution containing magnesium ion and iron ion is added drop-wise to be stirred continuously suspended In liquid, the nanometer galapectite pipe for being loaded with metal ion is centrifugally separating to obtain after dripping, wherein magnesium ion and iron ion is dense It is 2mol/L to spend, and the dripping quantity of nitrate is the 40% of suspension quality；Used silane coupler modified again, obtained after drying Ion modification nanometer galapectite pipe.
5) dry：Figured type superfine fibre bass to being obtained after main impregnation is dried.Drying temperature setting is as follows：The One 85 DEG C of area, the second 105 DEG C of area, the 3rd 115 DEG C of area, the 4th 125 DEG C of area, the 5th 130 DEG C of area, the 6th 140 DEG C of area；Drying rate It is 5 meters/min.
6) Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed.Alkali reduction When, alkali concn is 8%, and steam box temperature is 92 DEG C, and speed is 5 meters/min, and washing water-carrying capacity is 1.4 tons/h.
7) stoking is dried：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long.Stoking goes out leather speed 5 meters/min of degree, temperature is set as：First 95 DEG C of area, the second 120 DEG C of area, the 3rd 122 DEG C of area, the 4th 125 DEG C of area, the 5th area 130 ℃。
8) buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking.Buffing interval gap is set as：First Interval gap 1.0mm, the mesh of abrasive band 200, second interval gap 0.8mm, the mesh of abrasive band 400,5 meters/min of speed.
9) dye.
10) drying and shaping, final finished product.
Embodiment 5
A kind of preparation method of aqueous figured type flame-proof environmental protection suede, comprises the following steps：
1) pre- impregnation：From figured type superfine fibre nonwoven cloth as raw material, the non-woven fabrics is by determining island sea-island composite fiber system , described determine island component in the sea-island composite fiber of island be PA6, and sea component is COPET；Island number is 100, determines island fabric of island-in-sea type ultra-fine Fibre number is 3.5dtex, and non-woven fabrics grammes per square metre is in 450g/cm2, density 0.20g/cm2.Figured type superfine fibre nonwoven cloth is existed Impregnation process 35min in modified wool fat liquor, then takes out non-woven fabrics and wipes unnecessary emulsion away, then by non-woven fabrics aqueous In advance containing carrying out pre- impregnation in immersion liquid.
Wherein, the modified wool fat liquor is made up of following parts by weight of component：35 parts of modified wool fat, 61 parts of water and 4 Part emulsifying agent composition；The preparation method of the modified wool fat is as follows：Lanolin is heated in liquid, then in heat preservation strip Part lower used time 45min is to the phosphorus pentoxide that its quality 6% is at the uniform velocity added in lanolin；After reaction terminates, liquid is adjusted with alkali lye Body is neutrality, and modified wool fat is obtained after drying.
It is described aqueous pre- to be made up of following parts by weight of component containing immersion liquid：45 parts of waterborne polyurethane resin AE-12,155 parts of water.
2) dry：Non-woven fabrics after pre- impregnation is dried.Drying temperature setting is as follows：First 95 DEG C of area, the secondth area 110 DEG C, the 3rd 115 DEG C of area, the 4th 130 DEG C of area, the 5th 135 DEG C of area, drying rate：6 meters/min.
3) contracting is scalded：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting.It is 1.2mm to scald compression roller gap, and temperature is 125 DEG C, speed is 6 meters/min.
4) main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, the ultra-fine fibre of figured type is obtained Dimension bass；Aqueous master includes the component of following weight portion containing immersion liquid：0.15 part of aqueous color, 35 parts of water, 35 parts of aqueous polyurethanes Resin A E-12,5 parts of nanometer galapectite pipes, 1 part of aqueous dispersion AR-312,8 parts of halogen-free type fireproof powder Exolit op935,6 parts PA halogen-free environment-friendlyflame flame retardant Exolit op1240,0.1 part of defoamer.
The nanometer galapectite pipe is processed by ion modification, and method is as follows：Nanometer galapectite pipe is dispersed in water shape Into the suspension that mass concentration is 15%；Nitrate solution containing magnesium ion and iron ion is added drop-wise to be stirred continuously suspended In liquid, the nanometer galapectite pipe for being loaded with metal ion is centrifugally separating to obtain after dripping, wherein magnesium ion and iron ion is dense It is 1.5mol/L to spend, and the dripping quantity of nitrate is the 25% of suspension quality；Used silane coupler modified again, after drying To ion modification nanometer galapectite pipe.
5) dry：Figured type superfine fibre bass to being obtained after main impregnation is dried.Drying temperature setting is as follows：The One 95 DEG C of area, the second 100 DEG C of area, the 3rd 115 DEG C of area, the 4th 125 DEG C of area, the 5th 135 DEG C of area, the 6th 140 DEG C of area；Drying rate It is 6 meters/min.
6) Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed.Alkali reduction When, alkali concn is 9%, and steam box temperature is 95 DEG C, and speed is 6 meters/min, and washing water-carrying capacity is 1.8 tons/h.
7) stoking is dried：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long.Stoking goes out leather speed 6 meters/min of degree, temperature is set as：First 100 DEG C of area, the second 120 DEG C of area, the 3rd 125 DEG C of area, the 4th 130 DEG C of area, the 5th area 135℃。
8) buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking.Buffing interval gap is set as：First Interval gap 1.2mm, the mesh of abrasive band 250, second interval gap 1.0mm, the mesh of abrasive band 500,6 meters/min of speed.
9) dye.
10) drying and shaping, final finished product.
The obtained product of a present invention is chosen, choosing three positions (A, M, B) carries out performance test, and test result is such as Under：
Flame retardant test is carried out to suede of the invention, (instrument producer thinks carefully that electromechanics has in Nantong to tester model YG8150 Limit company), testing standard is GB8410, and test result is as follows：
Experiment one：Take the obtained suede of the present invention of three pieces of different parts；
Tested sample：10cmX30cmX3；
Test position：A/B/C；
Test result：A samples are less than 60mm/min；
B samples are less than 60mm/min；
C samples are less than 60mm/min.
Experiment two：Take three blocks of combustibles wrapped up with suede obtained in the present invention；
Tested sample：10cmX 30cmX3；
Test position：A/B/C；
Test result：A samples are less than 60mm/min；
B samples are less than 60mm/min；
C samples are less than 60mm/min.
Experiment three：Take three blocks of combustibles that conjunction is applied with the suede back side obtained in the present invention；
Tested sample：10cmX 30cmX3；
Test position：A/B/C；
Test result：A samples are less than 60mm/min；
B samples are less than 60mm/min；
C samples are less than 60mm/min.
From the foregoing, it will be observed that show that suede obtained in the present invention has very outstanding anti-flammability by fire-retardant experiment.
Raw materials used in the present invention, equipment, unless otherwise noted, is the conventional raw material, equipment of this area；In the present invention Method therefor, unless otherwise noted, is the conventional method of this area.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions, every according to the present invention Any simple modification, change and equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side The protection domain of case.

Claims (10)

1. a kind of preparation method of aqueous figured type flame-proof environmental protection suede, it is characterised in that comprise the following steps：
1）Pre- impregnation：By figured type superfine fibre nonwoven cloth in modified wool fat liquor impregnation process, then take out non-woven fabrics And wipe unnecessary emulsion away, then by non-woven fabrics it is aqueous it is pre- containing immersion liquid in carry out pre- impregnation；It is described it is aqueous it is pre- containing immersion liquid by following Parts by weight of component is constituted：35-45 parts of waterborne polyurethane resin, 155-165 parts of water；
2）Drying：Non-woven fabrics after pre- impregnation is dried；
3）Scald contracting：Non-woven fabrics after drying is entered into boiling hot compression roller carries out scalding contracting；
4）Main impregnation：Non-woven fabrics after boiling hot contracting is carried out into main impregnation in aqueous master contains immersion liquid, figured type superfine fibre shellfish is obtained This；Aqueous master includes the component of following weight portion containing immersion liquid：0.05-0.15 parts of aqueous color, 35-45 parts of water, 25-35 parts is aqueous Polyurethane resin, 3-5 parts of nanometer galapectite pipe, 1-2 parts of aqueous dispersion, 6-8 parts of halogen-free type fireproof powder, 6-8 parts of PA Halogen ring Environment friendly flame-retardant agent, 0.1-0.3 parts of defoamer；
5）Drying：Figured type superfine fibre bass to being obtained after main impregnation is dried；
6）Alkali reduction：Alkali reduction is carried out to the figured type superfine fibre bass after drying, is then washed；
7）Drying stoking：Figured type superfine fibre bass after Alkali reduction is carried out into line drying stoking long；
8）Buffing：Buffing is carried out to the figured type superfine fibre bass after drying stoking；
9）Dyeing；
10）Drying and shaping, final finished product.
2. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 1, it is characterised in that described Figured type superfine fibre nonwoven cloth is obtained by determining island sea-island composite fiber, it is described determine island sea-island composite fiber in island component be PA6, sea component is COPET；Island number is 30-180, and it is 0.5-5dtex to determine island sea-island composite fiber fiber number, and non-woven fabrics grammes per square metre exists 150-500g/cm2, density 0.16-0.22g/cm2.
3. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 1 or 2, it is characterised in that The modified wool fat liquor is made up of following parts by weight of component：25-35 parts of modified wool fat, 55-75 parts of water and 4-6 parts of emulsification Agent is constituted；The preparation method of the modified wool fat is as follows：Lanolin is heated to, in liquid, then to be used under heat-retaining condition When 40-50min to the phosphorus pentoxide that its quality 6-8% is at the uniform velocity added in lanolin；After reaction terminates, liquid is adjusted with alkali lye It is neutrality, modified wool fat is obtained after drying.
4. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 1 or 2, it is characterised in that Step 2）Drying temperature setting it is as follows：First 85-95 DEG C of area, the second 100-110 DEG C of area, the 3rd 110-120 DEG C of area, the 4th area 120-130 DEG C, the 5th 130-135 DEG C of area, drying rate：5-6 meters/min.
5. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 4, it is characterised in that step 3）Boiling hot compression roller gap be 0.8-1.4mm, temperature is 110-130oC, and speed is 5-6 meters/min.
6. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 1 or 2, it is characterised in that The nanometer galapectite pipe is processed by ion modification, and method is as follows：Nanometer galapectite pipe is dispersed in water to form quality dense Spend the suspension for 10-20%；Nitrate solution containing magnesium ion and iron ion is added drop-wise in the suspension being stirred continuously, The nanometer galapectite pipe for being loaded with metal ion is centrifugally separating to obtain after dripping, the wherein concentration of magnesium ion and iron ion is 1- 2mol/L, the dripping quantity of nitrate is the 20-40% of suspension quality；Used silane coupler modified again, dry after obtain from Sub- modified Nano galapectite pipe.
7. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 5, it is characterised in that step 5）Drying temperature setting it is as follows：First 85-95 DEG C of area, the second 100-110 DEG C of area, the 3rd 110-120 DEG C of area, the 4th area 120- 130 DEG C, the 5th 130-135 DEG C of area, the 6th 135-140 DEG C of area；Drying rate is 5-6 meters/min.
8. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 7, it is characterised in that step 6）Alkali reduction when, alkali concn is 7-10%, and steam box temperature is 90-95 DEG C, and speed is 5-6 meter/min, and washing water-carrying capacity is 1-2 Ton/h.
9. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 8, it is characterised in that step 7）In, stoking goes out to remove from office speed 5-6 meters/min, and temperature is set as：First 95-100 DEG C of area, the second 120-125 DEG C of area, the 3rd area 120-125 DEG C, the 4th 125-135 DEG C of area, the 5th 130-135 DEG C of area.
10. a kind of preparation method of aqueous figured type flame-proof environmental protection suede as claimed in claim 9, it is characterised in that step Rapid 8）In, buffing interval gap is set as：First interval gap 0.6-1.6 mm, abrasive band 180-320 mesh, second interval gap 0.4- 1.4mm, abrasive band 320-600 mesh, speed 5-6 meters/min.
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CN112593413B (en) * 2020-12-25 2021-12-31 四川大学 Preparation method of flame-retardant microfiber leather base cloth based on flame-retardant water-based polyurethane

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