CN108864405A - Air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin and preparation method thereof - Google Patents
Air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin and preparation method thereof Download PDFInfo
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- CN108864405A CN108864405A CN201810620372.2A CN201810620372A CN108864405A CN 108864405 A CN108864405 A CN 108864405A CN 201810620372 A CN201810620372 A CN 201810620372A CN 108864405 A CN108864405 A CN 108864405A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4816—Two or more polyethers of different physical or chemical nature mixtures of two or more polyetherpolyols having at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- 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
- D06N3/146—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 characterised by the macromolecular diols used
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- 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
- D06N3/147—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 characterised by the isocyanates used
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2205/00—Condition, form or state of the materials
- D06N2205/04—Foam
- D06N2205/045—Froth
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06N2209/00—Properties of the materials
- D06N2209/12—Permeability or impermeability properties
- D06N2209/121—Permeability to gases, adsorption
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- D06N2209/12—Permeability or impermeability properties
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- D06N2211/00—Specially adapted uses
- D06N2211/10—Clothing
- D06N2211/106—Footwear
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Abstract
The invention discloses a kind of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin and preparation method thereof, resin is made of hydroxy component A, isocyanate component B mixing；Hydroxy component A is high activity polyether dihydric alcohol（30-50 parts）, high activity polyether trihydroxylic alcohol（25-45 parts）, low molecular polyether dihydric alcohol（5-15 parts）, low molecular polyether trihydroxylic alcohol（5-10 parts）, chain extender（5-10 parts）, foaming agent（0.3-0.8 parts）, silicone oil auxiliary agent（0.1-0.5 parts）, catalyst（0.2-0.5 parts）；Isocyanate component B is polyisocyanates（40-60 parts）, high activity polyether dihydric alcohol（40-60 parts）, catalyst（0.1-0.3 parts）；The present invention also provides the preparation methods of the resin, and are applied in shoe lining leather manufacturing process, and DMF content is low, and breathable moisture permeability is good.
Description
Technical field
The present invention relates to chemical products and preparation method thereof technical field, specifically a kind of air-moisture-permeable shoe lining leather is with without molten
Agent Polyurethane Interlayer resin and preparation method thereof.
Background technique
Environmental requirement with global Synthetic Leather industry and consumer to synthetic leather product, eco-environmental prote have become
For one of the Basic Physical Properties of Synthetic Leather, either sofa furniture leather, luggage leather, interior leather for automobiles or sports shoe leather
Deng, be required to product DMF content control in 1000ppm hereinafter, some even require must not exceed 20ppm.And shoe lining leather, by
In it directly with the characteristic of human contact, higher to its eco-environmental prote requirement, moreover, shoe lining leather product is to ventilative saturating
Wet performance also has special strict demand.Therefore, production and processing raw material of the resin of environment-friendly type as shoe lining leather need to be selected,
Waterborne polyurethane resin and solvent-free polyurethane resin are comparatively ideal selection among these.
And compared with waterborne polyurethane resin, solvent-free polyurethane resin has more in terms of mechanical property and power consumption of polymer processing
Good advantage, therefore in recent years, as intermediate layer resin, it is studied ground more extensively and profoundly.But it is so far, there is not yet related
The shoe lining leather report of no-solvent polyurethane intermediate layer resin and preparation method thereof, especially shoe lining leather have breathable moisture permeability
There is higher requirement, common solvent-free polyurethane resin is difficult to meet this physical property.Therefore, it develops a with air-moisture-permeable
The shoe lining leather of performance no-solvent polyurethane intermediate layer resin, has great importance, and can satisfy the demand in market.
The object of the present invention is to provide a kind of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resins for summary of the invention
And preparation method thereof, it is unable to satisfy what shoe lining leather required breathable moisture permeability to solve prior art solvent-free polyurethane resin
Problem.
In order to achieve the above object, the technical scheme adopted by the invention is as follows：
Air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：By hydroxy component A, isocyanates group
Divide B according to mass ratio 1.5:1-1:1.5 are mixed with, wherein：
The hydroxy component A is made of the raw material of following parts by weight：
30-50 parts of high activity polyether dihydric alcohol,
25-45 parts of high activity polyether trihydroxylic alcohol,
5-15 parts of low molecular polyether dihydric alcohol,
5-10 parts of low molecular polyether trihydroxylic alcohol,
5-10 parts of chain extender,
0.3-0.8 parts of foaming agent,
0.1-0.5 parts of silicone oil auxiliary agent,
0.2-0.5 parts of catalyst,
The isocyanate component B is made of the raw material of following parts by weight：
40-60 parts of isocyanates,
40-60 parts of high activity polyether dihydric alcohol,
0.1-0.3 parts of catalyst.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The hydroxy component A
In, polyethylene glycol oxide-propylene oxide that high activity polyether dihydric alcohol is molecular weight 3000-6000 is copolymerized dihydric alcohol, polyoxyethylene
Alkene-propylene oxide copolymerization dihydric alcohol is made by ethylene oxide, propylene oxide as raw material copolymerization, ethylene oxide
Content account for ethylene oxide, propylene oxide total amount 20% or more；
Polyethylene glycol oxide-propylene oxide that high activity polyether trihydroxylic alcohol is molecular weight 3000-5000 is copolymerized trihydroxylic alcohol, polyoxyethylene
Alkene-propylene oxide copolymerization trihydroxylic alcohol is made by ethylene oxide, propylene oxide as raw material copolymerization, ethylene oxide
Content account for ethylene oxide, propylene oxide total amount 20% or more.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The hydroxy component A
In, low molecular polyether dihydric alcohol is the polyoxyethylene glycol of molecular weight 400-1000；Low molecular polyether trihydroxylic alcohol is
The polypropylene oxide trihydroxylic alcohol of molecular weight 400-1000.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The hydroxy component A
In, chain extender mixes composition according to mass ratio 9/1-7/3 with dihydromethyl propionic acid or dimethylolpropionic acid for ethylene glycol.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The hydroxy component A
In, foaming agent is chemical foaming agent, preferably water.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The hydroxy component A
In, silicone oil auxiliary agent is Siloxane-Oxyalkylene Copolymers.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The isocyanates
In component B, one or more of isocyanates MDI, MDI-50, Carbodiimide-Modified MDI are mixed by any mass ratio
Composition.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The isocyanates
In component B, high activity polyether dihydric alcohol is the polyoxyethylene glycol of molecular weight 1000-3000.
The air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：The hydroxy component A
It is organo-metallic catalyst with the catalyst in isocyanate component B, including but not limited to BiCAT 8108, BiCAT
3228、BiCAT 4232、Borchi Kat 22、Borchi Kat 24、MB20。
A kind of preparation method of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, which is characterized in that including
Following steps：
（1）, hydroxy component A preparation：By high activity polyether dihydric alcohol, high activity polyether trihydroxylic alcohol, low molecular polyether binary
Alcohol, low molecular polyether trihydroxylic alcohol, chain extender are put into reaction kettle, and stirring is warming up to 60-80 DEG C, and foaming agent, measurement is added
Moisture content is cooled to 30-40 DEG C after detection is qualified and silicone oil auxiliary agent, catalyst is added, stir evenly, mixture hydroxyl is made
Component A, sealed package are stand-by；
（2）The preparation of isocyanate component B：Isocyanates is put into reaction kettle and stirred evenly, high activity is then put into
Polyether Glycols and catalyst are simultaneously warming up to 60-90 DEG C, are stirred to react 2-4h and detect to NCO content qualified, are cooled to 30-50
DEG C, isocyanate component B is made, sealed package is stand-by；
（3）The preparation of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin：It is coated in release paper aqueous or without molten
Dosage form polyurethane cover slurry obtains polyurethane cover coating after drying forming；By obtained hydroxy component A, isocyanates
Component B is according to mass ratio 1.5:1-1:1.5 are sufficiently mixed, and then uniformly casting is applied coated on above-mentioned with polyurethane cover
In the release paper of layer, air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin can be prepared by 100-150 DEG C of drying.
No-solvent polyurethane intermediate layer resin produced by the present invention will be applied in the processing and manufacturing of shoe lining leather product,
Synthetic leather products DMF content is lower than 5ppm, breathable moisture permeability（Examination criteria：QB/T 1811-1993）Up to 2 mg/h*cm2
More than.
Compared with prior art, the present invention has following obvious advantage：
（1）The invention patent reports a kind of solvent-free polyurethane resin with breathable moisture permeability for the first time, is applied to shoe lining
When removing from office product processing, shoe lining leather product breathable moisture permeability obtained is good, and ecological, environmental protective performance is excellent, and snugness of fit is excellent；
（2）Resin of the present invention uses based on the polyether polyol of high EO content, and tree has not only been effectively ensured in the presence of EO group
The moisture-penetrable ventilated performance of rouge, and intensity is high compared to PO group, it is good with aqueous covercoat associativity, it can effectively avoid aqueous covercoat
The easy lamination problem in interface between resin and solvent-free middle layer polyurethane resin；
（3）The chain extender that resin of the present invention uses is ethylene glycol and dihydromethyl propionic acid or dimethylolpropionic acid according to certain matter
On the one hand amount is destroyed the crystallinity of hard section by chain extender blending method, the hardness of hard section is reduced, to improve than mixing composition
Shoe lining leather finished leather feel；On the other hand the chain extender for participating in being blended is dihydromethyl propionic acid or dihydroxymethyl containing carboxylic group
Butyric acid, by the introducing of the carboxylate radical with certain breathable moisture permeability, caused by can avoid introducing other chain extenders
The problem of moisture-penetrable ventilated performance of hard section declines；
（4）The silicone oil auxiliary agent that resin of the present invention uses for polyether-modified polysiloxanes, to resin formula provide dispersion performance,
While flow leveling, aperture performance, certain breathable moisture permeability is additionally provided, further ensures the saturating of resin of the present invention
Green permeability energy；
（5）The polyethylene glycol raw material of the excellent molecular weight 1000-3000 of the breathable moisture permeability that resin of the present invention introduces, is first logical
Synthesizing isocyanate performed polymer isocyanate component B is crossed, moisture-penetrable ventilated performance then is made with hydroxy component A material hybrid reaction again
Excellent solventfree resin, rather than polyethylene glycol raw material is introduced directly into component A formula；On the one hand, by synthesizing isocyanic acid
Ester performed polymer, can effectively avoid polyethylene glycol and may absorb water during storage causes to go bad, and influences asking for end product quality
Topic；On the other hand, it may cause hydroxy component A moisture if avoiding and being introduced into all polyethylene glycol in A material with blending method
Content changes, so that formulation ratio fluctuates when production and processing, influences production stability and end product quality
The problem of.
Specific embodiment
Below will by several specific embodiments, the present invention is further illustrated, it is to be noted that this hair
Specific material proportion, process conditions and result etc. described in bright embodiment are merely to illustrate the present invention, can not be with
This is limited the scope of the invention, and equivalent change or modification made by all Spirit Essences according to the present invention should all be contained
Lid is within the scope of the present invention.
Embodiment 1：
A kind of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, by hydroxy component A, isocyanate component B according to
Mass ratio 1.5:1 mixing composition；
The hydroxy component A is made of the raw material of following parts by weight：
High activity polyether dihydric alcohol（DP-3050E）30 parts
High activity polyether trihydroxylic alcohol（GY-5020E）45 parts
Low molecular polyether dihydric alcohol（DE-400）5 parts
Low molecular polyether trihydroxylic alcohol（GY-1000）10 parts
Chain extender（EG）9 parts
Chain extender（DMPA）1 part
Foaming agent（Deionized water）0.3 part
Silicone oil auxiliary agent（L-1160）0.5 part
Catalyst（BiCAT 8108）0.5 part
The isocyanate component B is made of the raw material of following parts by weight：
Isocyanates（MDI）50 parts
Isocyanates（MDI-50）10 parts
High activity polyether dihydric alcohol（DE-1000）40 parts
Catalyst（BiCAT 8108）0.1 part
DP-3050E in hydroxy component A is the high activity polyether two of the molecular weight 3000 of Kunshan national capital Chemical Co., Ltd. production
First alcohol, GY-5020E are the high activity polyether trihydroxylic alcohol of the molecular weight 5000 of Kunshan national capital Chemical Co., Ltd. production, DE-400
For the polyethylene dihydric alcohol of the molecular weight 400 of Kunshan national capital Chemical Co., Ltd. production, GY-1000 is that Kunshan national capital chemical industry is limited
The polypropylene trihydroxylic alcohol of the molecular weight 1000 of company's production, EG are commercial product, and DMPA is Sweden Perstorp speciality chemical
The dihydromethyl propionic acid of company's production, L-1160 are the primary hydroxyl Siloxane-Oxyalkylene Copolymers of Mai Tu company of U.S. production, BiCAT
8108 organic bismuth catalysts produced for the leading chemical company in the U.S..
MDI in isocyanate component B is the pure diphenylmethylene diisocyanate of Yantai Wanhua company production, MDI-50
It is the 4 of the production of Yantai Wanhua company, the mixture of 4 '-MDI and 2,4 '-MDI, DE-1000 are Kunshan national capital Chemical Co., Ltd.
The polyethylene dihydric alcohol of the molecular weight 1000 of production, BiCAT 8108 are the organo-bismuth catalysis of the leading chemical company production in the U.S.
Agent.
The present invention also provides the preparation method of above-mentioned air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, packets
Include following steps：
（1）The preparation of hydroxy component A：By high activity polyether dihydric alcohol DP-3050E, high activity polyether trihydroxylic alcohol GY-5020E, low
Molecular weight polyether dihydric alcohol DE-400, low molecular polyether trihydroxylic alcohol GY-1000, chain extender EG, chain extender DMPA are put into instead
It answers in kettle, stirring is warming up to 60 DEG C, and foaming agent deionized water is added, and measures moisture content, is cooled to 30 DEG C simultaneously after detection is qualified
Silicone oil auxiliary agent L-1160, catalyst BiCAT 8108 is added, stirs evenly, mixture A is made, sealed package is stand-by；
（2）The preparation of isocyanate component B：Isocyanates MDI and MDI-50 are put into reaction kettle and stirred evenly, then
Investment high activity polyether dihydric alcohol DE-1000 and catalyst BiCAT 8108 is simultaneously warming up to 60 DEG C, is stirred to react 4h to NCO content
Detection is qualified, is cooled to 30 DEG C, and component B is made, and sealed package is stand-by；
（3）The preparation of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin：It is coated in release paper aqueous or without molten
Dosage form polyurethane cover slurry obtains polyurethane cover coating after drying forming；By obtained hydroxy component A, isocyanates
Component B is according to mass ratio 1.5:1 is sufficiently mixed, then uniformly casting be coated on it is above-mentioned with polyurethane cover coating from
On type paper, air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin can be prepared by 100 DEG C of drying.
No-solvent polyurethane intermediate layer resin obtained above, is applied to shoe lining leather product, and resultant Leather can not will test DMF
（I.e. DMF content is lower than 5ppm）, breathable moisture permeability index（Examination criteria：QB/T 1811-1993）For 2.5 mg/h*cm2。
Embodiment 2：
A kind of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, by hydroxy component A, isocyanate component B according to
Mass ratio 1:1.5 mixing compositions；
The hydroxy component A is made of the raw material of following parts by weight：
High activity polyether dihydric alcohol（DP-6000E）50 parts
High activity polyether trihydroxylic alcohol（GY-3000E）25 parts
Low molecular polyether dihydric alcohol（DE-1000）15 parts
Low molecular polyether trihydroxylic alcohol（GY-420）5 parts
Chain extender（EG）3.5 part
Chain extender（DMPA）1.5 part
Foaming agent（Deionized water）0.8 part
Silicone oil auxiliary agent（L-1160）0.1 part
Catalyst（Borchi Kat 24）0.2 part
The isocyanate component B is made of the raw material of following parts by weight：
Isocyanates（MDI）35 parts
Isocyanates（MDI-100LL）5 parts
High activity polyether dihydric alcohol（DE-3000）60 parts
Catalyst（Borchi Kat 24）0.3 part
DP-6000E in hydroxy component A is the high activity polyether two of the molecular weight 6000 of Kunshan national capital Chemical Co., Ltd. production
First alcohol, GY-3000E are the high activity polyether trihydroxylic alcohol of the molecular weight 3000 of Kunshan national capital Chemical Co., Ltd. production, DE-1000
For the polyethylene dihydric alcohol of the molecular weight 1000 of Kunshan national capital Chemical Co., Ltd. production, GY-420 is that Kunshan national capital chemical industry is limited
The polypropylene trihydroxylic alcohol of the molecular weight 420 of company's production, EG are commercial product, and DMPA is that Sweden Perstorp speciality chemical is public
The dihydromethyl propionic acid of production is taken charge of, L-1160 is the primary hydroxyl Siloxane-Oxyalkylene Copolymers of Mai Tu company of U.S. production, Borchi
Kat 24 is the zinc polycarboxylate class catalyst of OMG Borchers company production.
MDI in isocyanate component B is the pure diphenylmethylene diisocyanate of Yantai Wanhua company production, MDI-
100LL is the diphenylmethylene diisocyanate of the Carbodiimide-Modified of Yantai Wanhua company production, and DE-3000 is Kunshan state
Polyethylene dihydric alcohols of the molecular weight 3000 of Chemical Co., Ltd.'s production, Borchi Kat 24 are OMG Borchers company
The zinc polycarboxylate class catalyst of production.
The present invention also provides the preparation method of above-mentioned air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, packets
Include following steps：
（1）The preparation of hydroxy component A：By high activity polyether dihydric alcohol DP-6000E, high activity polyether trihydroxylic alcohol GY-3000E, low
Molecular weight polyether dihydric alcohol DE-1000, low molecular polyether trihydroxylic alcohol GY-420, chain extender EG, chain extender DMPA are put into instead
It answers in kettle, stirring is warming up to 80 DEG C, and foaming agent deionized water is added, and measures moisture content, is cooled to 40 DEG C simultaneously after detection is qualified
Silicone oil auxiliary agent L-1160, catalyst Borchi Kat 24 is added, stirs evenly, mixture A is made, sealed package is stand-by；
（2）The preparation of isocyanate component B：Isocyanates MDI and MDI-100LL are put into reaction kettle and are stirred evenly,
Then it puts into high activity polyether dihydric alcohol DE-3000 and catalyst Borchi Kat 24 and is warming up to 90 DEG C, be stirred to react 2h extremely
NCO content detection is qualified, is cooled to 50 DEG C, and component B is made, and sealed package is stand-by；
（3）The preparation of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin：It is coated in release paper aqueous or without molten
Dosage form polyurethane cover slurry obtains polyurethane cover coating after drying forming；By obtained hydroxy component A, isocyanates
Component B is according to mass ratio 1:1.5 are sufficiently mixed, then uniformly casting be coated on it is above-mentioned with polyurethane cover coating from
On type paper, air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin can be prepared by 150 DEG C of drying.
No-solvent polyurethane intermediate layer resin obtained above, is applied to shoe lining leather product, can not will test DMF
（I.e. DMF content is lower than 5ppm）, breathable moisture permeability index（Examination criteria：QB/T 1811-1993）For 2.8 mg/h*cm2。
Embodiment 3：
A kind of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, by hydroxy component A, isocyanate component B according to
Mass ratio 1:1 mixing composition；
The hydroxy component A is made of the raw material of following parts by weight：
High activity polyether dihydric alcohol（DP-4000E）40 parts
High activity polyether trihydroxylic alcohol（GY-5020E）35 parts
Low molecular polyether dihydric alcohol（DE-700）10 parts
Low molecular polyether trihydroxylic alcohol（GY-700）7 parts
Chain extender（EG）6.5 part
Chain extender（DMBA）1.5 part
Foaming agent（Deionized water）0.5 part
Silicone oil auxiliary agent（L-1160）0.3 part
Catalyst（MB20）0.3 part
The isocyanate component B is made of the raw material of following parts by weight：
Isocyanates（MDI）50 parts
High activity polyether dihydric alcohol（DE-2000）50 parts
Catalyst（MB20）0.2 part
DP-4000E in hydroxy component A is the high activity polyether two of the molecular weight 4000 of Kunshan national capital Chemical Co., Ltd. production
First alcohol, GY-5020E are the high activity polyether trihydroxylic alcohol of the molecular weight 5000 of Kunshan national capital Chemical Co., Ltd. production, DE-700
For the polyethylene dihydric alcohol of the molecular weight 700 of Kunshan national capital Chemical Co., Ltd. production, GY-700 is that Kunshan national capital chemical industry is limited
The polypropylene trihydroxylic alcohol of the molecular weight 700 of company's production, EG are commercial product, and DMPA is that Sweden Perstorp speciality chemical is public
The dimethylolpropionic acid of production is taken charge of, L-1160 is the primary hydroxyl Siloxane-Oxyalkylene Copolymers of Mai Tu company of U.S. production, and MB20 is
The organic bismuth catalyst of air chemical company of U.S. production.
MDI in isocyanate component B is the pure diphenylmethylene diisocyanate of Yantai Wanhua company production, DE-
The polyethylene dihydric alcohol of 2000 molecular weight 2000 produced for Kunshan national capital Chemical Co., Ltd., MB20 are that US Air gasification work is public
Take charge of the organic bismuth catalyst of production.
The present invention also provides the preparation method of above-mentioned air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, packets
Include following steps：
（1）The preparation of hydroxy component A：By high activity polyether dihydric alcohol DP-4000E, high activity polyether trihydroxylic alcohol GY-5020E, low
Molecular weight polyether dihydric alcohol DE-700, low molecular polyether trihydroxylic alcohol GY-700, chain extender EG, chain extender DMBA put into reaction
In kettle, stirring is warming up to 70 DEG C, and foaming agent deionized water is added, and measures moisture content, and 35 DEG C are cooled to after detection is qualified and is added
Enter silicone oil auxiliary agent L-1160, catalyst MB20, stir evenly, mixture A is made, sealed package is stand-by；
（2）The preparation of isocyanate component B：Isocyanates MDI is put into reaction kettle and stirred evenly, then investment is high living
Property polyether Glycols DE-2000 and catalyst MB20 and be warming up to 80 DEG C, be stirred to react 3h and detect qualified, cooling to NCO content
To 40 DEG C, component B is made, sealed package is stand-by；
（3）The preparation of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin：It is coated in release paper aqueous or without molten
Dosage form polyurethane cover slurry obtains polyurethane cover coating after drying forming；By obtained hydroxy component A, isocyanates
Component B is according to mass ratio 1:1 is sufficiently mixed, and is then uniformly poured coated on above-mentioned release with polyurethane cover coating
On paper, air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin can be prepared by 130 DEG C of drying.
No-solvent polyurethane intermediate layer resin obtained above, is applied to shoe lining leather product, can not will test DMF
（I.e. DMF content is lower than 5ppm）, breathable moisture permeability index（Examination criteria：QB/T 1811-1993）For 3 mg/h*cm2。
Claims (10)
1. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin, it is characterised in that：By hydroxy component A, isocyanates
Component B is according to mass ratio 1.5:1-1:1.5 are mixed with, wherein：
The hydroxy component A is made of the raw material of following parts by weight：
30-50 parts of high activity polyether dihydric alcohol,
25-45 parts of high activity polyether trihydroxylic alcohol,
5-15 parts of low molecular polyether dihydric alcohol,
5-10 parts of low molecular polyether trihydroxylic alcohol,
5-10 parts of chain extender,
0.3-0.8 parts of foaming agent,
0.1-0.5 parts of silicone oil auxiliary agent,
0.2-0.5 parts of catalyst,
The isocyanate component B is made of the raw material of following parts by weight：
40-60 parts of isocyanates,
40-60 parts of high activity polyether dihydric alcohol,
0.1-0.3 parts of catalyst.
2. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in hydroxy component A, polyethylene glycol oxide-propylene oxide that high activity polyether dihydric alcohol is molecular weight 3000-6000 is copolymerized binary
Alcohol, polyethylene glycol oxide-propylene oxide copolymerization dihydric alcohol are made by ethylene oxide, propylene oxide as raw material copolymerization,
The content of ethylene oxide account for ethylene oxide, propylene oxide total amount 20% or more；
Polyethylene glycol oxide-propylene oxide that high activity polyether trihydroxylic alcohol is molecular weight 3000-5000 is copolymerized trihydroxylic alcohol, polyoxyethylene
Alkene-propylene oxide copolymerization trihydroxylic alcohol is made by ethylene oxide, propylene oxide as raw material copolymerization, ethylene oxide
Content account for ethylene oxide, propylene oxide total amount 20% or more.
3. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in hydroxy component A, low molecular polyether dihydric alcohol is the polyoxyethylene glycol of molecular weight 400-1000；Low molecular weight is poly-
Ether trihydroxylic alcohol is the polypropylene oxide trihydroxylic alcohol of molecular weight 400-1000.
4. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in hydroxy component A, chain extender is that ethylene glycol is mixed with dihydromethyl propionic acid or dimethylolpropionic acid according to mass ratio 9/1-7/3
Composition.
5. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in hydroxy component A, foaming agent is chemical foaming agent, preferably water.
6. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in hydroxy component A, silicone oil auxiliary agent is Siloxane-Oxyalkylene Copolymers.
7. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in isocyanate component B, one or more of isocyanates MDI, MDI-50, Carbodiimide-Modified MDI are by any
Mass ratio mixing composition.
8. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
It states in isocyanate component B, high activity polyether dihydric alcohol is the polyoxyethylene glycol of molecular weight 1000-3000.
9. air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin according to claim 1, it is characterised in that：Institute
Stating the catalyst in hydroxy component A and isocyanate component B is organo-metallic catalyst, including but not limited to BiCAT
8108、BiCAT 3228、BiCAT 4232、Borchi Kat 22、Borchi Kat 24、MB20。
10. a kind of if the described in any item air-moisture-permeable shoe lining leathers of claim 1-9 are with no-solvent polyurethane intermediate layer resin
Preparation method, which is characterized in that include the following steps：
（1）, hydroxy component A preparation：By high activity polyether dihydric alcohol, high activity polyether trihydroxylic alcohol, low molecular polyether binary
Alcohol, low molecular polyether trihydroxylic alcohol, chain extender are put into reaction kettle, and stirring is warming up to 60-80 DEG C, and foaming agent, measurement is added
Moisture content is cooled to 30-40 DEG C after detection is qualified and silicone oil auxiliary agent, catalyst is added, stir evenly, mixture hydroxyl is made
Component A, sealed package are stand-by；
（2）The preparation of isocyanate component B：Isocyanates is put into reaction kettle and stirred evenly, high activity is then put into
Polyether Glycols and catalyst are simultaneously warming up to 60-90 DEG C, are stirred to react 2-4h and detect to NCO content qualified, are cooled to 30-50
DEG C, isocyanate component B is made, sealed package is stand-by；
（3）The preparation of air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin：It is coated in release paper aqueous or without molten
Dosage form polyurethane cover slurry obtains polyurethane cover coating after drying forming；By obtained hydroxy component A, isocyanates
Component B is according to mass ratio 1.5:1-1:1.5 are sufficiently mixed, and then uniformly casting is applied coated on above-mentioned with polyurethane cover
In the release paper of layer, air-moisture-permeable shoe lining leather no-solvent polyurethane intermediate layer resin can be prepared by 100-150 DEG C of drying.
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| CN110066373B (en) * | 2019-03-19 | 2021-09-21 | 合肥科天水性科技有限责任公司 | Solvent-free polyurethane resin for synthetic leather, preparation method thereof and application of solvent-free polyurethane resin in water-based/solvent-free polyurethane synthetic leather |
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| WO2020203399A1 (en) * | 2019-03-29 | 2020-10-08 | 三井化学株式会社 | Foamed polyurethane resin composition, foamed polyurethane elastomer, and mid-sole |
| JPWO2020203399A1 (en) * | 2019-03-29 | 2021-10-21 | 三井化学株式会社 | Polyurethane foam resin composition, polyurethane foam elastomer and midsole |
| CN110951028A (en) * | 2019-11-12 | 2020-04-03 | 合肥科天水性科技有限责任公司 | Polyurethane resin and preparation method and application thereof |
| CN110951028B (en) * | 2019-11-12 | 2022-08-19 | 合肥科天水性科技有限责任公司 | Polyurethane resin and preparation method and application thereof |
| CN111072913A (en) * | 2019-11-26 | 2020-04-28 | 浙江禾欣科技有限公司 | Solvent-free polyurethane resin for automobile seat leather and preparation method thereof |
| CN111087574A (en) * | 2019-12-18 | 2020-05-01 | 福建成杰高分子材料有限公司 | Solvent-free middle layer polyurethane resin for synthetic leather and preparation method and application thereof |
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| CN112048054B (en) * | 2020-09-11 | 2022-01-07 | 浙江枧洋高分子科技有限公司 | Solvent type self-extinction moisture-permeable coating resin and preparation method thereof |
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| CN113307937B (en) * | 2021-05-26 | 2022-04-26 | 湖北祥源新材科技股份有限公司 | In-situ flame-retardant reinforced polyurethane foam and preparation method thereof |
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Application publication date: 20181123 |