CN102899918B - Method for producing wet-process waterborne polyurethane synthetic leather coating base - Google Patents
Method for producing wet-process waterborne polyurethane synthetic leather coating base Download PDFInfo
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- CN102899918B CN102899918B CN201210390119.5A CN201210390119A CN102899918B CN 102899918 B CN102899918 B CN 102899918B CN 201210390119 A CN201210390119 A CN 201210390119A CN 102899918 B CN102899918 B CN 102899918B
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Abstract
The invention relates to a method for producing a wet-process waterborne polyurethane synthetic leather coating base. The method comprises the following steps of: coating slurry on non-woven cloth by using a scraper of a blade coating machine in the coating amount of 80 to 380 g/m<2>; mixing 5 to 15 mass parts of demulsifier, 0.5 to 3 mass parts of cross-linking agent, 1 to 5 mass parts of 10 percent acid solution and 80 to 90 mass parts of water uniformly to obtain solidification liquid; allowing the non-woven cloth containing the coating slurry to pass through the solidification liquid; and washing the non-woven cloth, wringing and drying to obtain the wet-process waterborne polyurethane synthetic leather coating base. By the method, the problems of the pollution of a solvent of dimethylformamide and unsafety of products caused by dimethylformamide residues in the production of a solvent type wet-process polyurethane coating base can be solved; and the product has high physical and mechanical properties, water-vapor permeability and handfeel characteristics.
Description
Technical field
The present invention relates to Synthetic Leather technical field, particularly a kind of production method of aqueous polyurethane synthetic leather wet-process coating bass.
Background technology
Synthetic leather is institutional framework and the serviceability of simulation natural leather, and can be used as the composite of natural leather substitute.Conventionally with nonwoven fabric simulation lamina reticularis, with microvoid polyurethane coating simulation grain layer, resulting synthetic leather positive and negative are all quite similar with leather, and have certain gas permeability, than ordinary people fabricate-leather, more approach natural leather, be widely used in and make footwear, boots, case and bag and ball etc.
According to national statistics office data, show: the above enterprise of artificial leather synthetic leather scale (the new criteria for classifying: annual sales revenue 2000 ten thousand above enterprises) 495,2,410,000 tons of output, increase by 9.57% in 2011; 925.35 hundred million yuan of total industrial output values, increase by 29.55%; 69.85 hundred million yuan of profits taxes, increase by 32.12%; 47.86 hundred million yuan of total profits, increase by 36.15%.All in all, in the situation that the recovery of large economic environment, China's Synthetic Leather shows rapid growth momentum.
Bass, at synthetic leather industry middle finger semi-finished product, utilizes aqueous polyurethane synthetic leather wet-process coating bass, by the processing technology of follow-up routine, can produce all kinds of synthetic leather products.
At present, the production of Synthetic Leather wet-process coating bass mainly adopts solvent type production method, and its typical process flow is as follows: non-weaving cloth → blade coating → solidifying → washing → water squeezing → dry → coating bass.This production technology adopts solvent borne polyurethane, pigment and dimethyl formamide (DMF) for the coating paste that main component forms, and is first to utilize doctor knife coater to be coated on non-weaving cloth, then enters DMF and H
2o is in the solidification liquid of main component composition, due to solvent borne polyurethane and H
2o incompatible and DMF and H
2the unconfined of O dissolves each other, and makes solvent borne polyurethane/DMF system due to H
2the existence of O, DMF and H
2phase double replacement between O, makes DMF by H
2o extracts, and finally makes solvent borne polyurethane form micro porous coating, thereby obtains solvent borne polyurethane wet-process coating bass.This production method can produce two great problems, and the first has adopted DMF to make solvent, and process can cause the solvent contamination of DMF; It two is H
2o is the DMF in replacement solvent type polyurethane completely, can cause that the DMF of product is residual, finally causes product safety problem.
According to the production method of above-mentioned solvent borne polyurethane synthetic leather wet-process coating bass, production process exists serious DMF problem of environmental pollution, is a non-clean production process, and human body is had to larger harm.The residual product safety problem that causes that easily occurs DMF in resulting Synthetic Leather.
Summary of the invention
The production method that the object of this invention is to provide a kind of aqueous polyurethane synthetic leather wet-process coating bass, with solve DMF pollution problem that current solvent borne polyurethane synthetic leather wet-process coating bass produces in producing and synthetic leather produce in the residual product safety problem causing of product DMF.
For achieving the above object, the technical solution used in the present invention is:
Step 1, first, the aqueous gelatin solution that the aqueous pigment cream that the aqueous polyurethane that is 30% by 70～85 parts of solid contents by mass fraction, 5～10 parts of solid contents are 25% and 1～10 part of solid content are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, by doctor knife coater, coating paste is coated in to non-weaving cloth surface, the coating weight of coating paste is 80～380g/m
2;
Step 2, first, the acid solution that is 10% by 5～15 parts of demulsifiers, 0.5～3 part of crosslinking agent, 1～5 part of mass fraction by mass fraction and 80～90 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Then, the non-weaving cloth of the coating slurry of step 1, by solidification liquid, is formed to porous polyurethane coating;
Step 3, by the non-weaving cloth washing of step 2, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
It is the anion-type water-thinned polyurethane of carboxylate radical or sulfonate radical that described aqueous polyurethane adopts hydrophilic radical.
The water stain that described aqueous pigment cream adopts natural leather or synthetic leather suitability for industrialized production to use.
Described demulsifier is water-soluble magnesium salt, water-soluble Ca salt or water-soluble zinc salt.
Water-soluble magnesium salt is one or both in magnesium chloride, magnesium nitrate; Water-soluble Ca salt is one or both in calcium chloride, calcium nitrate; Water-soluble zinc salt is the mixture of one or more arbitrary proportions in zinc sulfate, zinc chloride, zinc acetate.
Described crosslinking agent is the mixture of one or more arbitrary proportions in aziridine, carbodiimides, trimethylol melamine, hexa methoxy methylene tri poly cyanamid.
Described acid solution is the mixture of one or more arbitrary proportions in formic acid, acetic acid, propionic acid, sulfuric acid, hydrochloric acid.
The coating paste temperature being coated in step 1 on non-weaving cloth is 20～50 ℃, and the solidification liquid temperature that in step 2, non-weaving cloth passes through is 20～80 ℃; The pH that is washed to aqueous polyurethane synthetic leather wet-process coating bass in step 3 is 6～7.
With respect to prior art, the present invention has following beneficial effect: use polyurethane coating slurry has replaced solvent borne polyurethane and DMF(dimethyl formamide) coating paste that forms, the solidification liquid that has replaced DMF and water to form with the solidification liquid that demulsifier, crosslinking agent, acid solution and water form, also just eliminate use and the pollution problem of DMF, also eliminated the product safety problem causing because DMF is residual in solvent borne polyurethane synthetic leather wet method bass simultaneously.The production environment of a safety can be provided, be of value to the healthy of workman; Resulting aqueous polyurethane synthetic leather wet-process coating bass is compared with solvent borne polyurethane synthetic leather wet-process coating bass, coating has the microcellular structure of very similar connection, and aqueous polyurethane synthetic leather wet-process coating bass has better physical and mechanical properties, gas permeability, water vapor permeability, moisture absorption hydrofuge and feel characteristic.
The specific embodiment
Below by the specific embodiment, the present invention is described in further detail, but the present invention has more than and is limited to these examples.
Embodiment 1:
Step 1, first, the hydrophilic radical that is 30% by 70 parts of solid contents by mass fraction is that the aqueous gelatin solution that the water stain that uses of natural leather suitability for industrialized production that the anion-type water-thinned polyurethane of carboxylate radical, 6 parts of solid contents are 25% and 2 parts of solid contents are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, the coating paste that is 20 ℃ by temperature by doctor knife coater is coated in non-weaving cloth surface, and the coating weight of coating paste is 200g/m
2;
Step 2, first, the formic acid that is 10% by 5 parts of demulsifier magnesium chlorides, 0.5 part of crosslinking agent aziridine, 1 part of mass fraction by mass fraction and 80 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Then, by the non-weaving cloth of the coating slurry of step 1, by temperature, be 40 ℃ of solidification liquids, form porous polyurethane coating;
Step 3, by the non-weaving cloth of step 2 be washed to that pH is 6, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
Embodiment 2:
Step 1, first, the hydrophilic radical that is 30% by 80 parts of solid contents by mass fraction is that the aqueous gelatin solution that the water stain that uses of synthetic leather suitability for industrialized production that the anion-type water-thinned polyurethane of sulfonate radical, 8 parts of solid contents are 25% and 7 parts of solid contents are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, the coating paste that is 40 ℃ by temperature by doctor knife coater is coated in non-weaving cloth surface, and the coating weight of coating paste is 160g/m
2;
Step 2, first, the acetic acid that is 10% by the mixture of 15 parts of demulsifier magnesium chlorides and magnesium nitrate, 2.5 parts of crosslinking agent carbodiimides, 5 parts of mass fractions by mass fraction and 90 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Then, by the non-weaving cloth of the coating slurry of step 1, by temperature, be 60 ℃ of solidification liquids, form porous polyurethane coating;
Step 3, by the non-weaving cloth of step 2 be washed to that pH is 7, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
Embodiment 3:
Step 1, first, the hydrophilic radical that is 30% by 72 parts of solid contents by mass fraction is that the aqueous gelatin solution that the water stain that uses of natural leather suitability for industrialized production that the anion-type water-thinned polyurethane of carboxylate radical, 5 parts of solid contents are 25% and 1 part of solid content are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, the coating paste that is 50 ℃ by temperature by doctor knife coater is coated in non-weaving cloth surface, and the coating weight of coating paste is 300g/m
2;
Step 2, first, the propionic acid that is 10% by 8 parts of demulsifier calcium chloride, 1 part of crosslinking agent trimethylol melamine, 2 parts of mass fractions by mass fraction and 83 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Then, by the non-weaving cloth of the coating slurry of step 1, by temperature, be 80 ℃ of solidification liquids, form porous polyurethane coating;
Step 3, by the non-weaving cloth of step 2 be washed to that pH is 6.5, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
Embodiment 4:
Step 1, first, the hydrophilic radical that is 30% by 75 parts of solid contents by mass fraction is that the aqueous gelatin solution that the water stain that uses of synthetic leather suitability for industrialized production that the anion-type water-thinned polyurethane of sulfonate radical, 7 parts of solid contents are 25% and 5 parts of solid contents are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, the coating paste that is 35 ℃ by temperature by doctor knife coater is coated in non-weaving cloth surface, and the coating weight of coating paste is 80g/m
2;
Step 2, first, the sulfuric acid that is 10% by the mixture of 10 parts of demulsifier calcium chloride and calcium nitrate, 2 parts of crosslinking agent hexa methoxy methylene tri poly cyanamids, 4 parts of mass fractions by mass fraction and 85 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Then, by the non-weaving cloth of the coating slurry of step 1, by temperature, be 20 ℃ of solidification liquids, form porous polyurethane coating;
Step 3, by the non-weaving cloth of step 2 be washed to that pH is 6.8, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
Embodiment 5:
Step 1, first, the hydrophilic radical that is 30% by 85 parts of solid contents by mass fraction is that the aqueous gelatin solution that the water stain that uses of natural leather suitability for industrialized production that the anion-type water-thinned polyurethane of carboxylate radical, 10 parts of solid contents are 25% and 10 parts of solid contents are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, the coating paste that is 45 ℃ by temperature by doctor knife coater is coated in non-weaving cloth surface, and the coating weight of coating paste is 140g/m
2;
Step 2, first, the hydrochloric acid that is 10% by the mixture of 12 parts of demulsifier zinc sulfate, 3 parts of crosslinking agent aziridine and carbodiimides, 5 parts of mass fractions by mass fraction and 88 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Then, by the non-weaving cloth of the coating slurry of step 1, by temperature, be 50 ℃ of solidification liquids, form porous polyurethane coating;
Step 3, by the non-weaving cloth of step 2 be washed to that pH is 6.3, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
Embodiment 6:
Step 1, first, the hydrophilic radical that is 30% by 83 parts of solid contents by mass fraction is that the aqueous gelatin solution that the water stain that uses of synthetic leather suitability for industrialized production that the anion-type water-thinned polyurethane of sulfonate radical, 9 parts of solid contents are 25% and 8 parts of solid contents are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, the coating paste that is 30 ℃ by temperature by doctor knife coater is coated in non-weaving cloth surface, and the coating weight of coating paste is 380g/m
2;
Step 2, first, the formic acid that is 10% by the mixture of the mixture of 13 parts of demulsifier zinc sulfate, zinc chloride and zinc acetate, 1.5 parts of crosslinking agent trimethylol melamines and hexa methoxy methylene tri poly cyanamid, 3 parts of mass fractions by mass fraction mixes and makes demulsifier dissolve to obtain solidification liquid completely with the mixture of hydrochloric acid and 86 parts of water;
Then, by the non-weaving cloth of the coating slurry of step 1, by temperature, be 70 ℃ of solidification liquids, form porous polyurethane coating;
Step 3, by the non-weaving cloth of step 2 be washed to that pH is 6.5, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
The non-weaving cloth that the present invention adopts is called again nonwoven fabric, can be various non-weaving cloths.
Key technology of the present invention and principle have following some:
One, the bright anion-type water-thinned polyurethane that utilizes of this law has replaced solvent borne polyurethane, in production process, can not use any solvent, can solve the DMF pollution problem producing in current solvent borne polyurethane synthetic leather wet-process coating bass production completely; Its two, the aqueous polyurethane synthetic leather wet-process coating bass that the present invention produces, containing DMF, can solve the safety problem causing because DMF is residual in current solvent borne polyurethane synthetic leather wet-process coating bass in product completely; Its three, owing to not using DMF, compare with the production of solvent borne polyurethane synthetic leather wet-process coating bass, save DMF removal process, whole energy-saving production technology consumption reduction; Its four, in whole production process, can not use any solvent, the production environment of a safety can be provided, be of value to the healthy of workman; They are five years old, resulting aqueous polyurethane synthetic leather wet-process coating bass is compared with solvent borne polyurethane synthetic leather wet-process coating bass, coating has the microcellular structure of very similar connection, and aqueous polyurethane synthetic leather wet-process coating bass has better physical and mechanical properties, gas permeability, water vapor permeability, moisture absorption hydrofuge and feel characteristic.
The aqueous gelatin solution adopting can play multiple effect, and one, can play good thickening power, makes coating paste reach the viscosity requirement of coating; Its two, can increase the thixotropy of coating paste, prevent the infiltration non-weaving cloth that coating paste is too much; Its three, can play and help freezing action, after making coating paste enter solidification liquid, solidify with speed faster on surface, thereby prevent that slurry is dispersed in solidification liquid; Its four, gelatin, under the effect of crosslinking agent, can form three-dimensional net structure, thereby improves the physical and mechanical properties of coating; Its five, gelatin is a kind of protide material, can improve flatness and the smooth feeling of coating.
After the non-weaving cloth of coating slurry immerses solidification liquid, one, the hydrogen ion (H that acid solution provides
+), by the hydrophilic radical carboxylate radical (in anion-type water-thinned polyurethane ?COO
-) and sulfonate radical (?SO
3 ?) be converted into carboxylate radical (?COOH) and sulfonate radical (?SO
3h), You Yu ?COOH Huo person ?SO
3hydrophily Yuan Yuan little Yu of H ?COO — He ?SO
3 ?so the stability of anion-type water-thinned polyurethane in the aqueous solution has decline; Its two, the CATION of demulsifier, i.e. divalence magnesium ion (Mg
2+), divalent calcium ion (Ca
2+), divalent zinc ion (Zn
2+) can further Feng Bi ?COO
-he ?SO
3 ?, the stability utmost point of anion-type water-thinned polyurethane in the aqueous solution reduced; Its three, crosslinking agent can and anion-type water-thinned polyurethane produce crosslinked action, the stability of reduction anionic soluble polyurethane in the aqueous solution.Under above-mentioned triple role, anion aqueous polyurethane breakdown of emulsion solidifies, and forms the polyurethane coating with microcellular structure.
Crosslinking agent has crosslinked ability to aqueous polyurethane, and aqueous polyurethane is thoroughly solidified, and improves the mechanical property of polyurethane gel coating.
Acid solution can regulate the pH of solidification liquid, and hydrogen ion (H is provided
+).
Resulting aqueous polyurethane synthetic leather wet-process coating bass is compared with solvent borne polyurethane synthetic leather wet-process coating bass, coating has the microcellular structure of very similar connection, and aqueous polyurethane synthetic leather wet-process coating bass has better physical and mechanical properties, gas permeability, water vapor permeability, moisture absorption hydrofuge and feel characteristic, refer to shown in table 1.
The key property contrast of two kinds of Synthetic Leather wet-process coating bass of table 1
Note: A sample is solvent borne polyurethane synthetic leather wet-process coating bass; B sample is aqueous polyurethane synthetic leather wet-process coating bass; A sample and B sample adopt same non-weaving cloth as base cloth.
Claims (6)
1. a production method for aqueous polyurethane synthetic leather wet-process coating bass, is characterized in that: comprise the following steps:
Step 1, first, the aqueous gelatin solution that the aqueous pigment cream that the aqueous polyurethane that is 30% by 70～85 parts of solid contents by mass fraction, 5～10 parts of solid contents are 25% and 1～10 part of solid content are 20% mixes, and through vacuumizing and defoaming, filtered through gauze, obtains coating paste;
Then, by doctor knife coater, coating paste is coated in to non-weaving cloth surface, the coating weight of coating paste is 80～380g/m
2;
Step 2, first, the acid solution that is 10% by 5～15 parts of demulsifiers, 0.5～3 part of crosslinking agent, 1～5 part of mass fraction by mass fraction and 80～90 parts of water mix and make demulsifier dissolve to obtain solidification liquid completely;
Described demulsifier is water-soluble magnesium salt, water-soluble Ca salt or water-soluble zinc salt, and wherein water-soluble magnesium salt is one or both in magnesium chloride, magnesium nitrate; Water-soluble Ca salt is one or both in calcium chloride, calcium nitrate; Water-soluble zinc salt is the mixture of one or more arbitrary proportions in zinc sulfate, zinc chloride, zinc acetate;
Then, the non-weaving cloth of the coating slurry of step 1, by solidification liquid, is formed to porous polyurethane coating;
Step 3, by the non-weaving cloth washing of step 2, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that to obtain.
2. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, is characterized in that: it is the anion-type water-thinned polyurethane of carboxylate radical or sulfonate radical that described aqueous polyurethane adopts hydrophilic radical.
3. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, is characterized in that: the water stain that described aqueous pigment cream adopts natural leather or synthetic leather suitability for industrialized production to use.
4. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, is characterized in that: described crosslinking agent is the mixture of one or more arbitrary proportions in aziridine, carbodiimides, trimethylol melamine, hexa methoxy methylene tri poly cyanamid.
5. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, is characterized in that: described acid solution is the mixture of one or more arbitrary proportions in formic acid, acetic acid, propionic acid, sulfuric acid, hydrochloric acid.
6. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, it is characterized in that: the coating paste temperature being coated in step 1 on non-weaving cloth is 20～50 ℃, the solidification liquid temperature that in step 2, non-weaving cloth passes through is 20～80 ℃; The pH that is washed to aqueous polyurethane synthetic leather wet-process coating bass in step 3 is 6～7.
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| CN201210390119.5A CN102899918B (en) | 2012-10-11 | 2012-10-11 | Method for producing wet-process waterborne polyurethane synthetic leather coating base |
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| CN201210390119.5A CN102899918B (en) | 2012-10-11 | 2012-10-11 | Method for producing wet-process waterborne polyurethane synthetic leather coating base |
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| CN104250939B (en) * | 2013-06-28 | 2016-07-06 | 桐乡市高桥皮革有限责任公司 | Finished leather is color-fixing method again |
| CN103981729B (en) * | 2014-05-07 | 2016-01-20 | 安安(中国)有限公司 | A kind of aqueous polyurethane for superfine fiber chemical leather manufacture makes face method |
| CN106917298B (en) * | 2017-04-21 | 2019-11-01 | 齐鲁工业大学 | A kind of preparation method of high color fastness dyeing-free superfine fiber chemical leather bass |
| CN108586692B (en) * | 2018-01-23 | 2020-09-22 | 陕西科技大学 | Preparation method and application of polishable waterborne polyurethane for synthetic leather |
| CN109680507B (en) * | 2018-07-23 | 2021-03-23 | 北华航天工业学院 | Application of lanthanum acetate and cerium acetate and preparation method of aqueous ecological synthetic leather wet-process bass |
| CN112300654B (en) * | 2019-07-26 | 2022-01-28 | 西牛皮防水科技有限公司 | Water-based rubber high-molecular waterproof coating and preparation method thereof |
| CN111041844A (en) * | 2019-12-24 | 2020-04-21 | 兰州科天水性高分子材料有限公司 | Anti-siphon shoe leather base and preparation method thereof |
| CN111286991A (en) * | 2020-03-19 | 2020-06-16 | 合肥科天水性科技有限责任公司 | Air filter medium and preparation method thereof |
| CN115961480A (en) * | 2022-12-27 | 2023-04-14 | 福建极利新材料科技有限公司 | Preparation method of waterborne polyurethane figured fiber bass |
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| JPH0291278A (en) * | 1988-09-29 | 1990-03-30 | Achilles Corp | Production of synthetic leather |
| JPH035110A (en) * | 1989-06-02 | 1991-01-10 | Ain Kk | Leather-patterned molding and its molding method |
| CN101705625A (en) * | 2009-10-14 | 2010-05-12 | 广东大盈化工有限公司 | Method for preparing leather by aqueous wet method |
| CN101717487A (en) * | 2009-11-20 | 2010-06-02 | 天津碧海蓝天水性高分子材料有限公司 | Polyurethane emulsion and coating agent used for aquosity coating agent of knitted lining glove as well as preparation method and coating method thereof |
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