CN115260438B - Preparation method of soft polyurethane elastomer - Google Patents
Preparation method of soft polyurethane elastomer Download PDFInfo
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- CN115260438B CN115260438B CN202210940306.XA CN202210940306A CN115260438B CN 115260438 B CN115260438 B CN 115260438B CN 202210940306 A CN202210940306 A CN 202210940306A CN 115260438 B CN115260438 B CN 115260438B
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- polyurethane elastomer
- polyol
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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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- 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
-
- 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
- C08G18/65—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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- 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
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
Abstract
The invention relates to a preparation method of a soft polyurethane elastomer, which comprises the following steps: the component B and the component A are mixed according to a proportion, poured into a mould at 80-100 ℃ for reaction, and vulcanized for 10-12 hours at 90-100 ℃. The preparation method of the component A comprises the following steps: mixing poly (propylene oxide) polyol and a micromolecular alcohol crosslinking agent in proportion, adding a catalyst with the concentration of 1000-1500ppm, and dehydrating at the temperature of 100-110 ℃ under the pressure of-0.1 MPa until the water content is less than or equal to 500ppm to obtain a component A; the preparation method of the component B comprises the following steps: 1, 5-pentanediisocyanate and polyether polyol with molecular weight of 1000 and hydroxyl value of 56mg KOH/g are mixed in proportion and reacted for 2-3 hours at 70-80 ℃ to obtain prepolymer with NCO content of 4-5 wt%. The prepared polyurethane elastomer has low hardness, soft touch feeling and good yellowing resistance, and is more suitable for the field with higher color requirements.
Description
Technical Field
The invention belongs to the field of polyurethane application, and particularly relates to a preparation method of an ultra-soft polyurethane elastomer.
Background
The polyurethane elastomer Young's model is between rubber and plastics, has excellent performances of wear resistance, oil resistance, tear resistance, chemical corrosion resistance, radiation resistance, good adhesion performance with materials, high elasticity, strong shock absorption and the like, and is widely applied to a plurality of fields of national economy. As polyurethane elastomers are increasingly used in flexible shoe materials, mobile phone housings, medical and packaging applications, there is an increasing demand for processability and flexibility. At present, the diisocyanate for synthesizing the super soft polyurethane elastomer is mainly aromatic diisocyanate, so two methods for increasing the molecular weight of the polyol in the soft segment of the polyurethane elastomer by adding a plasticizer or blending the plasticizer with other softer materials are mainly adopted in the way of improving the flexibility of the polyurethane elastomer. However, the mechanical and physical properties of the article are often reduced by the addition of plasticizers or blending with other softer materials and may even cause environmental problems. Meanwhile, due to the use of aromatic isocyanate, the yellowing resistance of the product is poor, and the product is unfavorable for being used in occasions with higher requirements on color. Therefore, the development of the ultra-soft polyurethane elastomer with yellowing resistance and good softness is very significant.
Disclosure of Invention
The invention aims to avoid the defects of the prior art and provides a preparation method of a soft polyurethane elastomer.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of a soft polyurethane elastomer is characterized in that: the method comprises the following specific steps:
the mass ratio of the component B to the component A is 100:10 to 100:20, controlling the temperature of the component B to be 60-70 ℃ and the temperature of the component A to be 35-40 ℃ when mixing, pouring the mixture into a mold at 80-100 ℃ for reaction after uniform mixing, demolding for 20-25min, and vulcanizing for 10-12 hours at 90-100 ℃;
the component A is prepared by the following method: mixing poly (propylene oxide) polyol and a micromolecular alcohol crosslinking agent in proportion, adding a catalyst with the concentration of 1000-1500ppm, and dehydrating at the temperature of 100-110 ℃ under the pressure of-0.1 MPa until the water content is less than or equal to 500ppm to obtain a component A;
the component B is prepared by the following method: 1, 5-pentanediisocyanate and polyether polyol with molecular weight of 1000 and hydroxyl value of 56mg KOH/g are mixed in proportion and reacted for 2-3 hours at 70-80 ℃ to obtain prepolymer with NCO content of 4-5 wt%.
In the component A, the mixture ratio of the poly (propylene oxide) polyol and the micromolecular alcohol cross-linking agent is as follows by mass percent: 65-70 wt% of polypropylene oxide polyol and 30-35 wt% of small molecular alcohol cross-linking agent.
In the component B, the proportion of the 1, 5-pentanediol and the polyether polyol is as follows by mass percent: 15-20-wt% of 1, 5-pentanediisocyanate and 80-wt-85-wt% of polyether polyol.
The polypropylene oxide ether polyol in the component A has the functionality of 2, the number average molecular weight of 2000 and the hydroxyl value of 107-117mg KOH/g.
The small molecular alcohol cross-linking agent in the component A is 1, 4-butanediol, and the catalyst is stannous octoate.
The beneficial effects of the invention are as follows: the polyurethane elastomer obtained by adopting the 1, 5-pentanediisocyanate as the isocyanate component and not adding other plasticizers has low hardness, soft touch and good yellowing resistance, and is more suitable for the field with higher requirements on the chromaticity and the flexibility of products.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
Preparing a component A: 650g of polypropylene oxide ether polyol, 350g of 1, 4-butanediol, 1.5g of stannous octoate as catalyst, and dehydrating to a water content of 470ppm at 100 ℃ and-0.1 MPa.
And (3) preparing a component B: 200g of 1, 5-pentanediisocyanate, 800g of polyether polyol having a molecular weight of 1000 and a hydroxyl value of 56mg KOH/g, and reacted at 80℃for 2 hours to give a prepolymer having an NCO content of 4.96% by weight.
The mass ratio of the component B to the component A is 100:10, controlling the temperature of the component B to 70 ℃, controlling the temperature of the component A to 35 ℃, uniformly mixing, pouring into a mold at 80 ℃ for reaction, demolding for 20min, and vulcanizing at 95 ℃ for 12 hours.
The properties were analyzed, hardness (Shore A) 40, elongation 1000% and rebound 42%.
Example 2
Preparing a component A: polypropylene oxide ether polyol 700g,1, 4-butanediol 300g, stannous octoate catalyst 1.0g, dehydrated to water content 430ppm at 110 deg.c, -0.1 MPa.
And (3) preparing a component B: 150g of 1, 5-pentanediisocyanate, 850g of polyether polyol with a molecular weight of 1000 and a hydroxyl value of 56mg KOH/g, and reacting at 70 ℃ for 3 hours to obtain a prepolymer with an NCO content of 4.12% by weight.
The mass ratio of the component B to the component A is 100:20, controlling the temperature of the component B to be 60 ℃, controlling the temperature of the component A to be 40 ℃, pouring the mixture into a mould at 100 ℃ for reaction after mixing, demoulding for 25min, and vulcanizing at 100 ℃ for 10 hours.
The properties were analyzed, hardness (Shore A) 38, elongation 1060% and rebound 43%.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (4)
1. A preparation method of a soft polyurethane elastomer is characterized in that: the method comprises the following specific steps:
the mass ratio of the component B to the component A is 100:10 to 100:20, controlling the temperature of the component B to be 60-70 ℃ and the temperature of the component A to be 35-40 ℃ when mixing, pouring the mixture into a mold at 80-100 ℃ for reaction after uniform mixing, demolding for 20-25min, and vulcanizing for 10-12 hours at 90-100 ℃;
the component A is prepared by the following method: mixing poly (propylene oxide) polyol and a micromolecular alcohol crosslinking agent in proportion, adding a catalyst with the concentration of 1000-1500ppm, and dehydrating at the temperature of 100-110 ℃ under the pressure of-0.1 MPa until the water content is less than or equal to 500ppm to obtain a component A;
the component B is prepared by the following method: 1, 5-pentanediisocyanate and polyether polyol with molecular weight of 1000 and hydroxyl value of 56mg KOH/g are mixed in proportion and reacted for 2-3 hours at 70-80 ℃ to obtain prepolymer with NCO content of 4-5 wt%.
2. The method for producing a flexible polyurethane elastomer according to claim 1, characterized in that: in the component A, the mixture ratio of the poly (propylene oxide) polyol and the micromolecular alcohol cross-linking agent is as follows by mass percent: 65-70 wt% of poly (propylene oxide) polyol and 30-35 wt% of small molecular alcohol cross-linking agent;
in the component B, the proportion of the 1, 5-pentanediol and the polyether polyol is as follows by mass percent: 15-20-wt% of 1, 5-pentanediisocyanate and 80-wt-85-wt% of polyether polyol.
3. A process for the preparation of a flexible polyurethane elastomer according to claim 1 or 2, characterized in that: the polypropylene oxide ether polyol in the component A has the functionality of 2, the number average molecular weight of 2000 and the hydroxyl value of 107-117mg KOH/g.
4. A process for the preparation of a flexible polyurethane elastomer according to claim 1 or 2, characterized in that: the small molecular alcohol cross-linking agent in the component A is 1, 4-butanediol, and the catalyst is stannous octoate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210940306.XA CN115260438B (en) | 2022-08-05 | 2022-08-05 | Preparation method of soft polyurethane elastomer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210940306.XA CN115260438B (en) | 2022-08-05 | 2022-08-05 | Preparation method of soft polyurethane elastomer |
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| CN115260438A CN115260438A (en) | 2022-11-01 |
| CN115260438B true CN115260438B (en) | 2023-08-29 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153393A (en) * | 2015-08-04 | 2015-12-16 | 李明莹 | Hydrophilic and biological safe polymer foam, and preparation method and application of polymer foam |
| CN107686550A (en) * | 2017-07-20 | 2018-02-13 | 青岛科技大学 | One kind is without plasticizer, soft, high elongation rate of tensile failure polyurethane elastomer material composition and preparation method thereof |
| EP3378880A1 (en) * | 2017-03-22 | 2018-09-26 | Covestro Deutschland AG | Porous materials based on a polyurethane polyisocyanurate mixture or a polyurea polyisocyanurate mixture and their production and use |
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2022
- 2022-08-05 CN CN202210940306.XA patent/CN115260438B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153393A (en) * | 2015-08-04 | 2015-12-16 | 李明莹 | Hydrophilic and biological safe polymer foam, and preparation method and application of polymer foam |
| EP3378880A1 (en) * | 2017-03-22 | 2018-09-26 | Covestro Deutschland AG | Porous materials based on a polyurethane polyisocyanurate mixture or a polyurea polyisocyanurate mixture and their production and use |
| CN107686550A (en) * | 2017-07-20 | 2018-02-13 | 青岛科技大学 | One kind is without plasticizer, soft, high elongation rate of tensile failure polyurethane elastomer material composition and preparation method thereof |
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| CN115260438A (en) | 2022-11-01 |
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