CN112661931A - Waterborne polyurethane resin for filling and preparation method thereof - Google Patents
Waterborne polyurethane resin for filling and preparation method thereof Download PDFInfo
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- CN112661931A CN112661931A CN202011528475.XA CN202011528475A CN112661931A CN 112661931 A CN112661931 A CN 112661931A CN 202011528475 A CN202011528475 A CN 202011528475A CN 112661931 A CN112661931 A CN 112661931A
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- 229920005749 polyurethane resin Polymers 0.000 title claims abstract description 49
- 238000011049 filling Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000004970 Chain extender Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- -1 diisocyanate compound Chemical class 0.000 claims abstract description 5
- 239000002562 thickening agent Substances 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000000839 emulsion Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 18
- 238000010559 graft polymerization reaction Methods 0.000 claims description 17
- 238000006116 polymerization reaction Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 230000001804 emulsifying effect Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 230000000149 penetrating effect Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002023 wood Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229920002635 polyurethane Polymers 0.000 claims description 5
- 239000004814 polyurethane Substances 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 125000005442 diisocyanate group Chemical group 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 3
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000010985 leather Substances 0.000 abstract description 22
- 239000002649 leather substitute Substances 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 231100000053 low toxicity Toxicity 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000004744 fabric Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 210000002257 embryonic structure Anatomy 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Abstract
The waterborne polyurethane resin for filling comprises the following components in parts by weight: 600 parts of polypropylene glycol, 180 parts of diisocyanate compound, 20-30 parts of dimethylolbutyric acid, 0.1-0.3 part of catalyst, 30-40 parts of acetone, 20-30 parts of chain extender, 10-18 parts of neutralizer and 1200 parts of deionized water. The product of the invention has the advantages of environmental protection, low toxicity, low VOC and the like. The softness of the filled leather is 2.5-3.0mm, and the softness of the synthetic leather is 4.0 mm. The waterborne polyurethane resin for filling prepared by the method can meet the requirements of industrial leather after being applied in a leather factory and a synthetic leather factory.
Description
Technical Field
The invention belongs to the field of leather spraying adhesives, and particularly relates to a waterborne polyurethane resin for filling and a preparation method thereof.
Background
After the original leather is treated by a leather tannery, the leather blank is divided into a first layer leather and a second layer leather, and the second layer leather is generally hard and has insufficient flexibility in the application process. For better utilization of the two-layered embryos, the embryos are usually filled with retanning fatliquoring, but this has limitations. With the increase of environmental protection pressure, the water field requirements of leather factories are more and more strict, and the improvement of the process is urgently needed. Similar problems are encountered when treating base fabrics in synthetic leather factories. The waterborne polyurethane resin for filling is researched in order to meet the environmental protection requirement and the market demand, and compared with a water field filler, the waterborne polyurethane resin for filling adopts water as a solvent, so that the environmental protection treatment pressure of a manufacturer is greatly reduced, the requirement of environmental protection is met, and the investment of water field equipment, sewage and the like can be reduced. The product of the invention has the advantages of environmental protection, low toxicity, low VOC and the like. The leather is suitable for improving the softness of the leather blank and the base cloth and simultaneously improving the hand feeling saturation of the leather blank and the base cloth. At present, the softness of leather is 2.5-3.0mm, and the softness of synthetic leather is 4.0 mm. Can completely meet the requirement of the market on softness.
Disclosure of Invention
The invention provides a filling waterborne polyurethane resin, which is used for overcoming the defects in the prior art.
The invention is realized by the following technical scheme:
the filling waterborne polyurethane resin comprises the following substances in parts by weight:
600 parts of polypropylene glycol, 180 parts of diisocyanate compound, 20-30 parts of dimethylolbutyric acid, 0.1-0.3 part of catalyst, 30-40 parts of acetone, 20-30 parts of chain extender, 10-18 parts of neutralizer and 1200 parts of deionized water.
The filling aqueous polyurethane resin as described above, wherein the molecular weight of the polypropylene glycol is 2000.
In the above-mentioned aqueous filling polyurethane resin, the diisocyanate compound is one or two of hexamethylene diisocyanate and toluene diisocyanate mixed at an arbitrary ratio.
The waterborne polyurethane resin for filling is characterized in that the catalyst is organic bismuth.
The filling waterborne polyurethane resin is characterized in that the chain extender is any one or two of 1, 6-hexanediol, neopentyl glycol, piperazine and ethylenediamine which are mixed in any proportion.
The filling aqueous polyurethane resin is characterized in that any one or two of the neutralizer N, N-dimethylethanolamine and triethylamine is mixed in any proportion.
The application method of the waterborne polyurethane resin emulsion for filling comprises the following steps: preparing an aqueous polyurethane resin emulsion: penetrant: leveling agent: medium shear thickening agent: and (2) weighing the low-shear thickening agent, namely wood powder, at a ratio of 1000:2:2:0.5:1:1, namely the aqueous polyurethane resin emulsion, the penetrating agent, the leveling agent, the high-shear thickening agent and the low-shear thickening agent, adding the penetrating agent and the leveling agent into the aqueous polyurethane resin emulsion, uniformly stirring by using a mechanical stirring device, adding the medium-shear thickening agent and the low-shear thickening agent, and continuously uniformly stirring by using the mechanical stirring device to complete the preparation of the waterborne polyurethane for filling.
The filling water-based polyurethane resin is the penetrating agent of 2440.
The filling waterborne polyurethane resin has the leveling agent with the height of 450.
The filling aqueous polyurethane resin is characterized in that the medium shear thickening agent is WH 601.
The filling water-based polyurethane resin is characterized in that the low-shear thickening agent is WH 301.
The filling waterborne polyurethane resin is wood powder of 200 meshes.
A preparation method of a filling waterborne polyurethane resin comprises the following steps:
the method comprises the following steps: weighing polypropylene glycol by using an accurate weighing platform scale, transferring the polypropylene glycol into a dehydration reaction kettle, sealing and vacuumizing, dehydrating the polypropylene glycol for 1.5h under the conditions of negative pressure of-0.06 MPa and temperature of 120 ℃;
step two: transferring polypropylene glycol into a polymerization reaction kettle after dehydration is finished, cooling to below 60 ℃, accurately weighing diisocyanate compounds and catalysts, transferring the diisocyanate compounds and the catalysts into the polymerization reaction kettle, heating to 85 ℃, timing to perform preliminary polymerization reaction, and reacting for 1.5 h;
step three: after the primary polymerization reaction, carrying out cooling operation, after the temperature is reduced to below 55 ℃, adding an accurate amount of dimethylolbutyric acid and a catalyst into a polymerization reaction kettle, adding acetone to promote dissolution and reduce the viscosity of a polymer, heating to 75 ℃ to carry out graft polymerization reaction for 1.5h, and finishing the first step of graft polymerization reaction;
step four: and (3) cooling to 55 ℃ after the first-step graft polymerization reaction is finished, weighing an accurate amount of the front chain extender, adding the front chain extender into a polymerization reaction kettle, heating to 75 ℃ for graft polymerization reaction for 1.0h, and finishing the second-step graft polymerization reaction.
Step five: and cooling the prepolymer, transferring the prepolymer into an emulsifying kettle after the prepolymer is cooled to 55 ℃, and accurately metering by adopting the weighing scales of the reaction kettle. Determining the amount of a neutralizing agent added into an emulsifying kettle according to the weight and the neutralization degree, carrying out hydrophilic neutralization chain extension salifying reaction for 10min, adding deionized water, adding a rear chain extender after phase inversion is finished, and stirring and dispersing for 0.5 h;
step six: and after the reaction in the fifth step is finished, transferring the mixture in the emulsifying kettle to a distillation kettle, heating to 56-60 ℃, simultaneously starting a vacuum pump, heating and vacuumizing for 0.5h, and removing acetone to obtain the aqueous polyurethane resin emulsion.
The invention has the advantages that:
1. the product of the invention has the advantages of environmental protection, low toxicity, low VOC and the like. The softness of the filled leather is 2.5-3.0mm, and the softness of the synthetic leather is 4.0 mm. The waterborne polyurethane resin for filling prepared by the method can meet the requirements of industrial leather after being applied in a leather factory and a synthetic leather factory.
2. The filling material is used in the market, a rotary drum production process is generally used, the production cost, the equipment input cost and the subsequent wastewater treatment cost are greatly increased, the filling process adopted by the invention can reduce the cost in all aspects and simplify the production process, and the external popularization of the product is facilitated.
3. The requirement for VOC measurement is higher and higher in the existing production field of genuine leather and synthetic leather, the demand of the product for acetone is very small, the acetone is basically eliminated completely when acetone is removed in the later period, the measurement requirement of VOC of each industrial standard can be met, in addition, no adverse effect is caused to operators during production and field application, the product is easy to store safely, no potential risk is caused, and the obvious environment-friendly advantage is achieved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic diagram showing the results of detection in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method comprises the following steps: accurately weighing 576kg of polypropylene glycol by a reduction method, transferring the polypropylene glycol into a dehydration reaction kettle, sealing, vacuumizing, dehydrating the polypropylene glycol for 1.5h under the conditions of negative pressure of-0.06 MPa and temperature of 120 ℃;
step two: transferring polypropylene glycol into a polymerization reaction kettle after dehydration is finished, cooling to below 60 ℃, weighing 140kg of toluene diisocyanate and 0.18kg of organic bismuth, adding the toluene diisocyanate and the organic bismuth into the polymerization reaction kettle, heating to 85 ℃, timing to start preliminary prepolymerization reaction, and reacting for 1.5 h;
step three: after the reaction is finished, cooling to 55 ℃, adding 23.5kg of dimethylolbutyric acid and 40kg of acetone into a prepolymerization reaction kettle, heating to 75 ℃ to perform graft polymerization pre-reaction for 1.5h, and finishing the first step of graft polymerization reaction;
step four: and (3) after the first-step graft polymerization reaction is finished, cooling to 55 ℃, adding 9kg of neopentyl glycol serving as a front chain extender, heating to 75 ℃ for graft polymerization reaction for 1 hour, and finishing the second-step reaction.
Step five: cooling the prepolymer, transferring the prepolymer into an emulsifying kettle after the temperature is reduced to 55 ℃, adding 14kg of N, N-dimethylethanolamine into the emulsifying kettle, carrying out the hydrophilic neutralization chain extension salifying reaction in the third step, reacting for 10min, adding 1350kg of deionized water, adding 4kg of rear chain extender ethylenediamine after the phase inversion is finished, and continuously stirring and reacting for 0.5 h;
step six: and after the reaction in the fifth step is finished, transferring the mixture in the emulsifying kettle to a distillation kettle, heating to 56-60 ℃, simultaneously starting a vacuum pump, heating and vacuumizing for 0.5h, and removing acetone to obtain the waterborne polyurethane resin emulsion with the solid content of 35%. Detecting the film forming performance of the emulsion, wherein the film hardness is 15 Shore A; the tensile strength of the film is 1.8MPa, and the elongation at break of the film is 750%.
The application method of the aqueous polyurethane resin emulsion comprises the following steps: preparing an aqueous polyurethane resin emulsion: penetrant: leveling agent: medium shear thickening agent: and (2) weighing the low-shear thickening agent, namely wood powder, at a ratio of 1000:2:2:0.5:1:1, adding the penetrating agent and the leveling agent into the aqueous polyurethane resin emulsion, uniformly stirring by using a mechanical stirring device, adding the medium-shear thickening agent and the low-shear thickening agent, and continuously uniformly stirring by using the mechanical stirring device to complete the preparation of the aqueous polyurethane for filling.
Product inspection report:
the leather blank is filled by adopting a three-plate printing mode, the filling material loading amount is controlled to be 10 threads, the physical property detection is carried out after the leather blank is dried, the softness is 2.6mm, and the requirement of a manufacturer on the production of the leather blank is met.
Example 2
A preparation method of waterborne polyurethane for filling comprises the following steps:
the method comprises the following steps: accurately weighing 500kg of polypropylene glycol by adopting a reduction method, transferring the polypropylene glycol into a dehydration reaction kettle, sealing, vacuumizing, dehydrating the polypropylene glycol for 1.5h under the conditions of negative pressure of-0.06 MPa and temperature of 120 ℃;
step two: transferring polypropylene glycol into a polymerization reaction kettle after dehydration is finished, cooling to below 60 ℃, weighing 120kg of toluene diisocyanate and 10kg of hexamethylene diisocyanate, transferring the toluene diisocyanate and the hexamethylene diisocyanate into the polymerization reaction kettle, heating to 85 ℃, timing to perform a first-step prepolymerization reaction, and reacting for 1.5 h;
step three: after the reaction is finished, cooling to 55 ℃, adding 20kg of dimethylolbutyric acid and 30kg of acetone into a prepolymerization reaction kettle, heating to 75 ℃ to carry out graft polymerization pre-reaction for 1.5h, and finishing the first-step graft polymerization reaction;
step four: and (3) after the first-step graft polymerization reaction is finished, cooling to 55 ℃, adding 20kg of front chain extender 1.6 hexanediol, heating to 75 ℃ for polymerization reaction for 1h, and finishing the second-step reaction.
Step five: cooling the prepolymer, transferring the prepolymer into an emulsifying kettle after the temperature is reduced to 55 ℃, adding 13kg of triethylamine into the emulsifying kettle, carrying out the third step of hydrophilic neutralization chain extension salifying reaction for 0.5h, adding 1200kg of deionized water, adding 2kg of rear chain extender ethylenediamine after the phase inversion is finished, and continuously stirring for reaction for 0.5 h;
step six: and after the reaction in the fifth step is finished, transferring the mixture in the emulsifying kettle to a distillation kettle, heating to 56-60 ℃, simultaneously starting a vacuum pump, heating and vacuumizing for 0.5h, and removing acetone to obtain the waterborne polyurethane resin emulsion with the solid content of 34%. Detecting the film forming property of the emulsion, wherein the film hardness is 10 Shore A; the tensile strength of the film is 1.4MPa, and the elongation at break of the film is 800%.
The application method of the aqueous polyurethane resin emulsion comprises the following steps: preparing an aqueous polyurethane resin emulsion: penetrant: leveling agent: medium shear thickening agent: the low shear thickening agent is 1000:2:2:0.5: the preparation method comprises the following steps of 1, weighing the aqueous polyurethane resin emulsion, the penetrating agent, the leveling agent, the medium-shear thickening agent and the low-shear thickening agent according to a proportion, adding the penetrating agent and the leveling agent into the aqueous polyurethane resin emulsion, uniformly stirring by using a mechanical stirring device, adding the medium-shear thickening agent and the low-shear thickening agent, and continuously uniformly stirring by using the mechanical stirring device to complete the preparation of the aqueous polyurethane for filling.
And (3) performance detection:
and (3) filling the synthetic leather base cloth by adopting a three-plate printing mode, controlling the filling material loading amount to be 15 threads, detecting the physical property after drying, and meeting the requirement of a manufacturer on base cloth production, wherein the softness is 3.9 mm.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A filling aqueous polyurethane resin characterized by comprising: the composition comprises the following substances in parts by weight:
600 parts of polypropylene glycol, 180 parts of diisocyanate compound, 20-30 parts of dimethylolbutyric acid, 0.1-0.3 part of catalyst, 30-40 parts of acetone, 20-30 parts of chain extender, 10-18 parts of neutralizer and 1200 parts of deionized water.
2. The aqueous filling polyurethane resin according to claim 1, wherein: the molecular weight of the polypropylene glycol is 2000.
3. The aqueous filling polyurethane resin according to claim 1, wherein: the diisocyanate compound is any one or two of hexamethylene diisocyanate and toluene diisocyanate which are mixed in any proportion.
4. The aqueous filling polyurethane resin according to claim 1, wherein: the catalyst is organic bismuth.
5. The aqueous filling polyurethane resin according to claim 1, wherein: the chain extender is any one or two of 1, 6-hexanediol, neopentyl glycol, piperazine and ethylenediamine which are mixed in any proportion.
6. The aqueous filling polyurethane resin according to claim 1, wherein: any one or two of the neutralizer N, N-dimethylethanolamine and triethylamine is mixed in any proportion.
7. The aqueous filling polyurethane resin according to claim 1, wherein: the application method of the aqueous polyurethane resin emulsion comprises the following steps: preparing an aqueous polyurethane resin emulsion: penetrant: leveling agent: medium shear thickening agent: and (2) weighing the low-shear thickening agent, namely wood powder, at a ratio of 1000:2:2:0.5:1:1, namely the aqueous polyurethane resin emulsion, the penetrating agent, the leveling agent, the high-shear thickening agent and the low-shear thickening agent, adding the penetrating agent and the leveling agent into the aqueous polyurethane resin emulsion, uniformly stirring by using a mechanical stirring device, adding the medium-shear thickening agent and the low-shear thickening agent, and continuously uniformly stirring by using the mechanical stirring device to complete the preparation of the waterborne polyurethane for filling.
8. The aqueous filling polyurethane resin according to claim 1, wherein:
the penetrating agent is medium 2440;
the leveling agent is 450 mm high;
the medium shear thickening agent is WH 601;
the low-shear thickening agent is WH 301;
the wood powder is 200-mesh wood powder.
9. A method for preparing a filling waterborne polyurethane resin is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: weighing polypropylene glycol by using an accurate weighing platform scale, transferring the polypropylene glycol into a dehydration reaction kettle, sealing and vacuumizing, dehydrating the polypropylene glycol for 1.5h under the conditions of negative pressure of-0.06 MPa and temperature of 120 ℃;
step two: transferring polypropylene glycol into a polymerization reaction kettle after dehydration is finished, cooling to below 60 ℃, accurately weighing diisocyanate compounds and catalysts, transferring the diisocyanate compounds and the catalysts into the polymerization reaction kettle, heating to 85 ℃, timing to perform preliminary polymerization reaction, and reacting for 1.5 h;
step three: after the primary polymerization reaction, carrying out cooling operation, after the temperature is reduced to below 55 ℃, adding an accurate amount of dimethylolbutyric acid and a catalyst into a polymerization reaction kettle, adding acetone to promote dissolution and reduce the viscosity of a polymer, heating to 75 ℃ to carry out graft polymerization reaction for 1.5h, and finishing the first step of graft polymerization reaction;
step four: and (3) cooling to 55 ℃ after the first-step graft polymerization reaction is finished, weighing an accurate amount of the front chain extender, adding the front chain extender into a polymerization reaction kettle, heating to 75 ℃ for graft polymerization reaction for 1.0h, and finishing the second-step graft polymerization reaction.
Step five: and cooling the prepolymer, transferring the prepolymer into an emulsifying kettle after the prepolymer is cooled to 55 ℃, and accurately metering by adopting the weighing scales of the reaction kettle. Determining the amount of a neutralizing agent added into an emulsifying kettle according to the weight and the neutralization degree, carrying out hydrophilic neutralization chain extension salifying reaction for 10min, adding deionized water, adding a rear chain extender after phase inversion is finished, and stirring and dispersing for 0.5 h;
step six: and after the reaction in the fifth step is finished, transferring the mixture in the emulsifying kettle to a distillation kettle, heating to 56-60 ℃, simultaneously starting a vacuum pump, heating and vacuumizing for 0.5h, and removing acetone to obtain the aqueous polyurethane resin emulsion.
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| CN202011528475.XA CN112661931A (en) | 2020-12-22 | 2020-12-22 | Waterborne polyurethane resin for filling and preparation method thereof |
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| CN202011528475.XA CN112661931A (en) | 2020-12-22 | 2020-12-22 | Waterborne polyurethane resin for filling and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002033001A1 (en) * | 2000-10-17 | 2002-04-25 | Nanopol Inc. | Synthetic leather manufacturing method using aqueous polyurethane dispersions |
| EP2186839A1 (en) * | 2008-11-13 | 2010-05-19 | Bayer MaterialScience AG | Polyurethane dispersions for coating with barrier features |
| CN102070759A (en) * | 2010-11-29 | 2011-05-25 | 陕西科技大学 | Method for preparing water-based polyurethane leather retanning agent |
| CN103030769A (en) * | 2012-12-07 | 2013-04-10 | 青岛文创科技有限公司 | Polyurethane retanning filler |
| EP3816342A1 (en) * | 2019-10-30 | 2021-05-05 | Asahi Kasei Kabushiki Kaisha | Artificial leather and production method therefor |
-
2020
- 2020-12-22 CN CN202011528475.XA patent/CN112661931A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002033001A1 (en) * | 2000-10-17 | 2002-04-25 | Nanopol Inc. | Synthetic leather manufacturing method using aqueous polyurethane dispersions |
| EP2186839A1 (en) * | 2008-11-13 | 2010-05-19 | Bayer MaterialScience AG | Polyurethane dispersions for coating with barrier features |
| CN102070759A (en) * | 2010-11-29 | 2011-05-25 | 陕西科技大学 | Method for preparing water-based polyurethane leather retanning agent |
| CN103030769A (en) * | 2012-12-07 | 2013-04-10 | 青岛文创科技有限公司 | Polyurethane retanning filler |
| EP3816342A1 (en) * | 2019-10-30 | 2021-05-05 | Asahi Kasei Kabushiki Kaisha | Artificial leather and production method therefor |
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| Title |
|---|
| 刘益军: "《聚氨酯树脂及其应用》", 化学工业出版社 * |
| 强涛涛: "《合成革化学品》", 31 July 2016, 中国轻工业出版社 * |
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Application publication date: 20210416 |