CN109762323A - A kind of ultra-soft matter wet process buckling resin and its preparation method and application - Google Patents
A kind of ultra-soft matter wet process buckling resin and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to chemical products and preparation method thereof technical fields, and disclose a kind of ultra-soft matter wet process buckling resin and its preparation method and application, raw material including following weight kilogram number proportion: PE-1 is 50 kilograms, PE-2 is 50 kilograms, PE-3 is double centner, PCDL-2000 is 25 kilograms and DMF is 697 kilograms and (launches in two times, it is for the first time 300 kilograms, second of 397 kilograms of step by step input).A kind of ultra-soft matter wet process buckling resin and its preparation method and application, pass through the polycarbonate of selection collocation proper proportion, the high temperature resistance of resin can be greatly improved, it can prevent synthetic leather surface from burning while reaching buckling effect, by selecting the polyester of different molecular weight mashed up, reduce the symmetry of polyurethane molecular structure, there is better dissolubility compared with the done product of unimodal molecular weight polyester, and resistance to low temperature is good, resin appearance is limpider and transparent, by selecting other suitable long-chain chain extenders of ethylene glycol collocation on chain extender selects.
Description
Technical field
The present invention relates to chemical products and preparation method thereof technical field, specially a kind of ultra-soft matter wet process buckling resin and
Preparation method and application.
Background technique
Resin typically refer to it is heated after be softened or melted range, there are liquidity preference, room temperature in when softening under external force
Under be solid-state and semisolid, be also possible to the organic polymer of liquid sometimes, in a broad aspect, it is former to can be used as plastic products processing
Any high-molecular compound of material is referred to as resin, and relative molecular weight is uncertain but usually higher, is in solid-state, middle solid-state under room temperature
And pseudo-solid condition, it is also possible to the organic substance of liquid sometimes, has and be softened or melted temperature range, there is flowing under external force
Tendency, rupture are in conchoidal often, broadly refer to polymer or prepolymer as plastic basis material, general not soluble in water, energy
It is dissolved in organic solvent, can by sources be divided into natural resin and synthetic resin, has thermoplasticity again by the different feature of its processing behavior
Point of resin and thermosetting resin.
Tradition trade mark resin generally concentrates on neutralizing high hard at present, and that there are water washing effects is poor for a small number of soft trade mark resins,
Not heatproof is easy to burn even carbonization bass surface buckling at a lower temperature, and setting time is long, production efficiency one
As, so propose that a kind of ultra-soft matter wet process buckling resin and its preparation method and application solves the above problems.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of ultra-soft matter wet process buckling resin and preparation method thereof and answer
With solving the above problems, have the high temperature resistance for being effectively improved resin, while having good water washing effect again, surfacing,
The advantages that good at flesh, and buckling effect stability is uniform, it is poor to solve a small number of soft trade mark resins there are water washing effects, intolerant to
Temperature is easy to burn even carbonization bass surface buckling at a lower temperature, and setting time is long, and production efficiency is general
Problem.
(2) technical solution
To realize the above-mentioned high temperature resistance for being effectively improved resin, while there is good water washing effect again, surfacing, at
Flesh is good, and the uniform purpose of buckling effect stability, the invention provides the following technical scheme: a kind of ultra-soft matter wet process buckling resin and
Preparation method and application, the raw material including following weight kilogram number proportion: PE-1 is 50 kilograms, PE-2 is 50 kilograms, PE-3
Be 25 kilograms for double centner, PCDL-2000, DMF be 697 kilograms (launch in two times, be for the first time 300 kilograms, second by
Step investment 397 kilograms), EG be 4.4 kilograms, 16HD is 1.1 kilograms, phosphoric acid is 0.03 kilogram, antioxidant is 0.2 kilogram, MT is
57 kilograms, CATA be 0.2 kilogram, CH3OH is 0.5 kilogram, malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
Preferably, the PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and the PET-2 is AA-EG-BG:
2000 molecujar weight polyols.
Preferably, the PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and the CATA is catalyst.
Preferably, the PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and the DMF is dimethylformamide.
Preferably, the EG is ethylene glycol, and the 16HD is 16- hexylene glycol；The AH-01 is wax emulsion.
Another technical problem to be solved by the present invention is that provide a kind of ultra-soft matter wet process buckling resin and preparation method thereof and
Using, comprising the following steps:
1) PE-1, PET-2, PE-3, DMF, EG, 16HD, phosphoric acid, AH-01, antioxidant and MT are put into three-necked flask first
In be stirred；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled in 70-80
DEG C, and visual response speed conditions, CATA is added as one sees fit；
3) DMF is gradually added during thickening to be diluted, finally controls 180Pas-220Pas/25 DEG C of viscosity, be added
CH3OH is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent clarified solution that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C
Body；
(3) beneficial effect
Compared with prior art, the present invention provides a kind of ultra-soft matter wet process buckling resin and its preparation method and application,
Have it is following the utility model has the advantages that
1, ultra-soft matter wet process buckling resin and its preparation method and application passes through the poly- carbonic acid of selection collocation proper proportion
Ester can greatly improve the high temperature resistance of resin, can prevent synthetic leather surface from burning while reaching buckling effect, pass through
It selects the polyester of different molecular weight mashed up, the symmetry of polyurethane molecular structure is reduced, compared with the done product of unimodal molecular weight polyester
With better dissolubility, and resistance to low temperature is good, and resin appearance is limpider and transparent, by selecting on chain extender selects
Other suitable long-chain chain extenders of ethylene glycol collocation are selected, the symmetrical performance of polyurethane molecular can be reduced, molecule segment can be fitted
Intermolecular force between hard section can achieve ideal buckling effect under low temperature, selected by auxiliary agent so that softening point reduces
It is opposite not add auxiliary agent with tradition for the washing environmental protection wax emulsion that upper selection not only has anti-adhesion effects but also has hot pressure effect difunctional
Than, can the larger smooth degree for changing surface, and temperature needed for buckling can be reduced.
2, ultra-soft matter wet process buckling resin and its preparation method and application, prepares material and quantity by improvement, reaches
Setting time is shorter, so that throughput rate can be improved in leather making process, save the cost can be under the premise of identical materials
Higher thickness is obtained, so that more materials can be saved when producing same thickness product, due to adding for polycarbonate
Enter, the physical mechanical property of product can be greatly improved, it, can be with so that product peel strength promotes obvious, the addition of wax emulsion
Smooth degree is greatly improved, greatly improves soft Trademark leather and is easy tacky problem, takes different molecular weight polyalcohol mashed up and long
Chain and the mashed up formula design of short chain chain extender, can greatly reduce the regularity of molecule segment, reduce hydrogen in polyurethane molecular
The active force of key realizes to substantially reduce softening point and reaches ideal buckling effect at lower temperature, this can also be reduced
The introducing of the consumption of the energy, polycarbonate polyol can also make product obtain certain anti-hydrolytic performance, this is also a Xiang Yi
Outer harvest.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment one: a kind of ultra-soft matter wet process buckling resin and its preparation method and application, including following weight kilogram number
The raw material of proportion: PE-1 is double centner, PE-2 is 50 kilograms, PE-3 is 50 kilograms, PCDL-2000 is 25 kilograms, DMF 705
Kilogram (launch in two times, be for the first time 300 kilograms, second of 405 kilograms of step by step input), EG are 6.37 kilograms, 16HD is
1.59 kilograms, phosphoric acid be 0.03 kilogram, antioxidant is 0.5 kilogram, MT is 57.6 kilograms, CATA is 0.2 kilogram, CH3OH 0.5
Kilogram, malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and PET-2 is AA-EG-BG:2000 molecujar weight polyol.
PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and CATA is catalyst.
PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and DMF is dimethylformamide.
EG is ethylene glycol, and 16HD is 16- hexylene glycol；AH-01 is wax emulsion.
A kind of ultra-soft matter wet process buckling resin and its preparation method and application, comprising the following steps:
1) PE-1, PET-2, PE-3, DMF, EG, 16HD, phosphoric acid, AH-01, antioxidant and MT are put into three-necked flask first
In be stirred；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled in 70-80
DEG C, and visual response speed conditions, CATA is added as one sees fit；
3) DMF is gradually added during thickening to be diluted, finally controls 180Pas-220Pas/25 DEG C of viscosity, be added
CH3OH is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent clarified solution that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C
Body；
Embodiment two: a kind of ultra-soft matter wet process buckling resin and its preparation method and application, including following weight kilogram number
The raw material of proportion: PE-1 is double centner, PE-2 is 50 kilograms, PE-3 is 50 kilograms, PCDL-2000 is 25 kilograms, DMF 705
Kilogram (launch in two times, be for the first time 300 kilograms, second of 405 kilograms of step by step input), EG be 6.37 kilograms, DEG 1.63
Kilogram, phosphoric acid be 0.03 kilogram, antioxidant is 0.2 kilogram, MT is 57.7 kilograms, CATA is 0.2 kilogram, CH3OH is 0.5 thousand
Gram, malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and PET-2 is AA-EG-BG:2000 molecujar weight polyol.
PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and CATA is catalyst.
PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and DMF is dimethylformamide.
EG is ethylene glycol, and 16HD is 16- hexylene glycol；AH-01 is wax emulsion.
A kind of ultra-soft matter wet process buckling resin and its preparation method and application, comprising the following steps:
1) PE-1, PET-2, PE-3, DMF, EG, DEG, phosphoric acid, AH-01, antioxidant and MT are put into three-necked flask first
In be stirred；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled in 70-80
DEG C, and visual response speed conditions, CATA is added as one sees fit；
3) DMF is gradually added during thickening to be diluted, finally controls 180Pas-220Pas/25 DEG C of viscosity, be added
CH3OH is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent clarified solution that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C
Body；
Embodiment three: a kind of ultra-soft matter wet process buckling resin and its preparation method and application, including following weight kilogram number
The raw material of proportion: PE-1 is 1000 kilograms, PE-2 is 50 kilograms, PE-3 is 50 kilograms, PCDL-2000 is 25 kilograms, DMF is
705 kilograms (launch in two times, be for the first time 300 kilograms, second of 405 kilograms of step by step input), EG be 6.53 kilograms, 16HD is
1.63 kilograms, phosphoric acid be 0.03 kilogram, antioxidant is 0.2 kilogram, MT is 57.7 kilograms, CATA is 0.2 kilogram, CH3OH 0.5
Kilogram, malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and PET-2 is AA-EG-BG:2000 molecujar weight polyol.
PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and CATA is catalyst.
PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and DMF is dimethylformamide.
EG is ethylene glycol, and 16HD is 16- hexylene glycol；AH-01 is wax emulsion.
A kind of ultra-soft matter wet process buckling resin and its preparation method and application, comprising the following steps:
1) PE-1, PET-2, PE-3, DMF, EG, 16HD, phosphoric acid, AH-01, antioxidant and MT are put into three-necked flask first
In be stirred；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled in 70-80
DEG C, and visual response speed conditions, CATA is added as one sees fit；
3) DMF is gradually added during thickening to be diluted, finally controls 180Pas-220Pas/25 DEG C of viscosity, be added
CH3OH is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent clarified solution that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C
Body；
Example IV: a kind of ultra-soft matter wet process buckling resin and its preparation method and application, including following weight kilogram number
The raw material of proportion: PE-1 is 70 kilograms, PE-2 is 65 kilograms, PE-3 is 65 kilograms, PCDL-2000 is 25 kilograms, DMF 705
Kilogram (launch in two times, be for the first time 300 kilograms, second of 405 kilograms of step by step input), EG are 5.74 kilograms, 16HD is
1.43 kilograms, phosphoric acid be 0.03 kilogram, antioxidant is 0.2 kilogram, MT is 57.5 kilograms, CATA is 0.2 kilogram, CH3OH 0.5
Kilogram, malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and PET-2 is AA-EG-BG:2000 molecujar weight polyol.
PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and CATA is catalyst.
PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and DMF is dimethylformamide.
EG is ethylene glycol, and 16HD is 16- hexylene glycol；AH-01 is wax emulsion.
A kind of ultra-soft matter wet process buckling resin and its preparation method and application, comprising the following steps:
1) PE-1, PET-2, PE-3, DMF, EG, 16HD, phosphoric acid, AH-01, antioxidant and MT are put into three-necked flask first
In be stirred；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled in 70-80
DEG C, and visual response speed conditions, CATA is added as one sees fit；
3) DMF is gradually added during thickening to be diluted, finally controls 180Pas-220Pas/25 DEG C of viscosity, be added
CH3OH is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent clarified solution that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C
Body；
Embodiment five: a kind of ultra-soft matter wet process buckling resin and its preparation method and application, including following weight kilogram number
The raw material of proportion: PE-1 is 50 kilograms, PE-2 is 50 kilograms, PE-3 is double centner, PCDL-2000 is 25 kilograms, DMF 697
Kilogram (launch in two times, be for the first time 300 kilograms, second of 397 kilograms of step by step input), EG be 4.4 kilograms, 16HD 1.1
Kilogram, phosphoric acid be 0.03 kilogram, antioxidant is 0.2 kilogram, MT is 57 kilograms, CATA is 0.2 kilogram, CH3OH is 0.5 kilogram,
Malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and PET-2 is AA-EG-BG:2000 molecujar weight polyol.
PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and CATA is catalyst.
PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and DMF is dimethylformamide.
EG is ethylene glycol, and 16HD is 16- hexylene glycol；AH-01 is wax emulsion.
A kind of ultra-soft matter wet process buckling resin and its preparation method and application, comprising the following steps:
1) PE-1, PET-2, PE-3, DMF, EG, 16HD, phosphoric acid, AH-01, antioxidant and MT are put into three-necked flask first
In be stirred；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled in 70-80
DEG C, and visual response speed conditions, CATA is added as one sees fit；
3) DMF is gradually added during thickening to be diluted, finally controls 180Pas-220Pas/25 DEG C of viscosity, be added
CH3OH is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent clarified solution that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C
Body；
Judgment criteria: sentenced according to resin state, setting time, thickness, peel strength, discoloring temperature and surface slip degree
It is disconnected.
The beneficial effects of the present invention are: resin can be greatly improved by the polycarbonate of selection collocation proper proportion
High temperature resistance can prevent synthetic leather surface from burning while reaching buckling effect, by the polyester for selecting different molecular weight
It is mashed up, the symmetry of polyurethane molecular structure is reduced, there is better dissolubility compared with the done product of unimodal molecular weight polyester, and resistance to
Cryogenic property is good, and resin appearance is limpider and transparent, by chain extender selects select ethylene glycol arrange in pairs or groups it is suitable its
His long-chain chain extender, can reduce the symmetrical performance of polyurethane molecular, can fit intermolecular force between molecule segment hard section,
So that softening point reduces, ideal buckling effect can achieve under low temperature, select to select that both there are anti-adhesion effects by auxiliary agent
The washing environmental protection wax emulsion difunctional with hot pressure effect again, does not add auxiliary agent with tradition and compares, and larger can change surface
Smooth degree, and temperature needed for capable of reducing buckling, prepare material and quantity by improvement, and it is shorter to have reached setting time, so that
Can be improved throughput rate in leather making process, save the cost can obtain higher thickness under the premise of identical materials, so that
When producing same thickness product, more materials can be saved, due to the addition of polycarbonate, product can be greatly improved
Physical mechanical property so that product peel strength is promoted obvious, the addition of wax emulsion can greatly improve smooth degree, greatly
Improve soft Trademark leather and be easy tacky problem, takes different molecular weight polyalcohol mashed up mashed up with long-chain and short chain chain extender
Formula design, can greatly reduce the regularity of molecule segment, the active force of hydrogen bond in polyurethane molecular be reduced, to drop significantly
Low softening point realizes and reaches ideal buckling effect at lower temperature, this can also reduce the consumption of the energy, and polycarbonate is more
The introducing of first alcohol can also make product obtain certain anti-hydrolytic performance, this is also a windfall, solve a small number of soft
That there are water washing effects is poor for trade mark resin, not heatproof, is easy to burn even carbonization bass table buckling at a lower temperature
Face, setting time is long, the general problem of production efficiency.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of ultra-soft matter wet process buckling resin and its preparation method and application, which is characterized in that including following weight kilogram number
The raw material of proportion: PE-1 is 50 kilograms, PE-2 is 50 kilograms, PE-3 is double centner, PCDL-2000 is 25 kilograms, DMF 697
Kilogram (launch in two times, be for the first time 300 kilograms, second of 397 kilograms of step by step input), EG be 4.4 kilograms, 16HD 1.1
Kilogram, phosphoric acid be 0.03 kilogram, antioxidant is 0.2 kilogram, MT is 57 kilograms, CATA is 0.2 kilogram, CH3OH is 0.5 kilogram,
Malic acid is 0.3 kilogram and AH-01 is 10 kilograms.
2. a kind of ultra-soft matter wet process buckling resin according to claim 1 and its preparation method and application, which is characterized in that
The PE-1 is AA-EG-BG:4000 molecular weight polyisoprene ester polyol, and the PET-2 is AA-EG-BG:2000 molecujar weight polyol.
3. a kind of ultra-soft matter wet process buckling resin according to claim 1 and its preparation method and application, which is characterized in that
The PE-3 is AA-BG:1000 molecular weight polyisoprene ester polyol, and the CATA is catalyst.
4. a kind of ultra-soft matter wet process buckling resin according to claim 1 and its preparation method and application, which is characterized in that
The PCDL-2000 is 2000 molecular weight polycarbonate polyalcohols, and the DMF is dimethylformamide.
5. a kind of ultra-soft matter wet process buckling resin according to claim 1 and its preparation method and application, which is characterized in that
The EG is ethylene glycol, and the 16HD is 16- hexylene glycol；The AH-01 is wax emulsion.
6. a kind of ultra-soft matter wet process buckling resin and its preparation method and application, which comprises the following steps:
1) first by PE-1, PET-2, PE-3, DMF, EG, 16HD, phosphoric acid, AH-01, antioxidant and MT be put into three-necked flask into
Row stirring；
2) after mixing evenly, then PCDL-2000 is added in substep, it is made mutually to melt thickening, and reaction temperature is controlled at 70-80 DEG C, and
Visual response speed conditions, add CATA as one sees fit；
3) DMF being gradually added during thickening to be diluted, finally controlling 180Pas-220Pas/25 DEG C of viscosity, CH3OH is added
It is blocked；
4) it then puts into anti-visbreaking auxiliary agent malic acid to wait for stirring completely, uniformly rear cooling is poured into special plastic bottle；
5) finally obtaining solid content is 30% or so, the transparent supernatant liquid that viscosity is 100Pas/25 DEG C -140Pas/25 DEG C.
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Application publication date: 20190517 |