CN114591484A - Preparation method of non-foaming polyurethane elastomer with excellent mechanical property - Google Patents
Preparation method of non-foaming polyurethane elastomer with excellent mechanical property Download PDFInfo
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Abstract
The invention relates to a preparation method of a non-foaming polyurethane elastomer with excellent mechanical properties, belonging to the technical field of polyurethane elastomers. Uniformly mixing PTMEG 200070-71 parts, 330N 19-20 parts, BDO 7.3-7.5 parts, X-3131.8-2.0 parts and T-120.0003-0.002 part to prepare a component A; a prepolymer with NCO content of 12-13 percent formed by the reaction of isocyanate containing-NCO groups and PTMEG2000 is marked as a component B; the component A and the component B which are preheated to (30 +/-2) ° C are stirred and mixed for (25 +/-5) s at the rotating speed of 1900 rpm-2200 rpm, then the mixture is placed under the condition that the vacuum degree is less than or equal to 0.09MPa for vacuum defoamation for 8 min-10 min, then the mixture is placed into a mold preheated to (75 +/-5) ° C, then the mold is placed into an oven at (75 +/-5) ° C for curing for 1 h-1.5 h, and then the mold is cured at (25 +/-5) ° C for (48 +/-5) h, so that the non-foaming polyurethane elastomer with excellent mechanical property is obtained.
Description
Technical Field
The invention relates to a preparation method of a non-foaming polyurethane elastomer with excellent mechanical properties, belonging to the technical field of polyurethane elastomers.
Background
The polyurethane elastomer is an elastomer material with wide application, has the characteristics of excellent mechanical strength, toughness, wear resistance, oil resistance and the like due to wide selectivity of raw materials and a special microphase separation structure, and can be applied to many fields of shoe materials, pipes, films and sheets, cables, automobiles, buildings, medical sanitation, national defense and the like.
In the preparation process of the polyurethane elastomer, if foaming agents such as water and the like are added to prepare the foamed polyurethane elastomer, a large number of cellular structures exist in a product, so that the mechanical property is relatively poor, and the foamed polyurethane elastomer is mainly used for vibration reduction, noise reduction, heat preservation, heat insulation and the like; if no foaming agent is added, the non-foaming polyurethane elastomer is obtained, has excellent mechanical properties due to no foam holes and compact structure, and is mainly used in the fields of automobile parts, pipes, buildings and the like. However, the production process of the unfoamed polyurethane elastomer inevitably involves defects such as bubbles, and the gelation rate is high, so that the defoaming treatment before curing is not performed for a sufficient time, and the theoretical mechanical properties cannot be achieved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a non-foaming polyurethane elastomer with excellent mechanical properties, which controls the gelation reaction degree by regulating and controlling the content of each component, particularly strictly controlling the content of a catalyst and optimizing the process conditions of vacuum defoaming treatment at the same time, so that sufficient time is provided for defoaming treatment before forming, thereby effectively removing bubbles introduced in the preparation process, and further improving the strength and toughness of the non-foaming polyurethane elastomer without influencing other properties.
The purpose of the invention is realized by the following technical scheme.
A method for preparing a non-foaming polyurethane elastomer with excellent mechanical properties, which comprises the following steps:
the component A and the component B which are preheated to (30 +/-2) ° C are stirred and mixed for (25 +/-5) s at the rotating speed of 1900 rpm-2200 rpm, then the mixture is placed under the condition that the vacuum degree is less than or equal to 0.09MPa for vacuum defoamation for 8 min-10 min, then the mixture is placed into a mold preheated to (75 +/-5) ° C, then the mold is placed into an oven at (75 +/-5) ° C for curing for 1 h-1.5 h, and then the mold is cured at (25 +/-5) ° C for (48 +/-5) h, so that the non-foaming polyurethane elastomer with excellent mechanical property is obtained.
The component A is prepared by mixing polytetrahydrofuran ether glycol (PTMEG2000) with the molecular weight of 2000, polyoxypropylene triol (330N) with the molecular weight of 4950, 1, 4-Butanediol (BDO), an antifoaming agent with the model number of X-313 of New Material company, Guangzhou, Detian, and dibutyltin dilaurate (T-12); wherein the component A comprises the following components in parts by weight: PTMEG 200070-71 parts, 330N 19-20 parts, BDO 7.3-7.5 parts, X-3131.8-2.0 parts and T-120.0003-0.002 parts;
the component B is a prepolymer with NCO content of 12-13% formed by the reaction of isocyanate containing-NCO groups and PTMEG 2000;
in addition, the molar ratio of-OH groups in the component A to-NCO groups in the component B is (1.03-1.07): 1; the water content of PTMEG2000, 330N and BDO is less than or equal to 500 ppm.
And the component B is a prepolymer with NCO content of 12-13% formed by stirring and reacting (3.8-4.2) h of isocyanate containing-NCO groups and PTMEG2000 at the temperature of 80-85 ℃.
Further, the isocyanate having an — NCO group is 4, 4' -diphenylmethane diisocyanate (MDI); in this case, the components in the component B are as follows in parts by mass: PTMEG 200054-57 parts and MDI 44-47 parts.
Further, T-12 was dissolved in 330N and mixed with PTMEG2000, BDO and X-313.
Furthermore, the mass part of T-12 in the component A is 0.0003-0.0005.
Has the advantages that:
(1) the invention regulates the gelation reaction rate of the system by regulating the content of each component, particularly the content of the catalyst, optimizes the process parameters in the preparation process, avoids introducing bubbles in the preparation process as much as possible, and has enough time for defoaming treatment before molding to remove the introduced bubbles and reduce the defects of products, thereby obtaining the polyurethane elastomer which has almost no bubbles, high strength and good toughness.
(2) Because the influence of the content of the catalyst on the gelation rate of the reaction system is very large, the content of the catalyst is reduced as much as possible, and the content of the catalyst is too low to be controlled accurately, so that the invention firstly adds the low-content catalyst into the high-content 330N which is not reacted with the low-content catalyst for dilution, and then mixes the 330N containing the catalyst with the PTMEG2000, BDO and X-313, thereby realizing the accurate control of the low-content catalyst and having simple and convenient operation.
(3) The method provided by the invention is simple to operate, effectively reduces the defect of foam holes in the non-foaming polyurethane elastomer, enables the tensile strength of the prepared polyurethane elastomer to be more than or equal to 18MPa and the elongation at break to be more than 700%, and has a good application prospect.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of a tensile section of the non-foamed polyurethane elastomer prepared in example 1.
Fig. 2 is a surface scanning electron microscope image of the non-foamed polyurethane elastomer prepared in comparative example 1.
Fig. 3 is a surface scanning electron microscope image of the non-foamed polyurethane elastomer prepared in comparative example 2.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
Example 1
(1) Respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, the PTMEG 330N and the BDO until the water content is less than or equal to 500 ppm;
(2) dissolving 0.005 part of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; uniformly mixing 70.9 parts of dehydrated PTMEG2000, 19.7 parts of 330N containing T-12, 7.4 parts of dehydrated BDO and 1.9 parts of X-313 (a defoaming agent of a New Material company, Guangzhou, No. X-313) to obtain a component A;
uniformly mixing 45 parts of MDI and 55 parts of PTMEG under the nitrogen protection atmosphere, and stirring and reacting for 4 hours at 80-85 ℃ to obtain a prepolymer capped by-NCO, which is abbreviated as a component B and has the NCO content of 12.5%;
(3) respectively preheating the component A and the component B to 30 ℃, then mixing the preheated component A and the preheated component B according to the molar ratio of-OH groups in the component A to-NCO groups in the component B of 1.05, stirring and mixing for 30s at the rotating speed of 2000rpm, then placing the mixture in a vacuum degree of less than or equal to 0.09MPa for 10min, then placing the mixture in a mold preheated to 70 ℃, then placing the mold in an oven at 70 ℃ for curing for 1.5h, and then curing for 48h at 25 ℃ to obtain the unfoamed polyurethane elastomer with excellent mechanical properties.
The microstructure representation of the prepared non-foaming polyurethane elastomer is carried out, and as can be seen from the SEM picture in figure 1, the polyurethane elastomer has no obvious bubbles on the stretching section, which indicates that the defoaming is complete in the preparation process. The tensile strength and elongation at break of the prepared non-foamed polyurethane elastomer were tested with reference to the standard GB/T1040.3-2006, and the tensile strength of the polyurethane elastomer was 19.18MPa and the elongation at break was 782%.
Example 2
(1) Respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, the PTMEG 330N and the BDO until the water content is less than or equal to 500 ppm;
(2) dissolving 0.0045 part of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; uniformly mixing 70.8 parts of dehydrated PTMEG2000, 19.5 parts of 330N containing T-12, 7.5 parts of dehydrated BDO and 1.8 parts of X-313 (a defoaming agent of a New Material company, Guangzhou, No. X-313) to obtain a component A;
uniformly mixing 44 parts of MDI and 56 parts of PTMEG under the nitrogen protection atmosphere, and stirring and reacting for 4.2 hours at the temperature of 80-85 ℃ to obtain a prepolymer terminated by-NCO, which is abbreviated as a component B and has the NCO content of 12.6%;
(3) respectively preheating the component A and the component B to 28 ℃, then mixing the preheated component A and the preheated component B according to the molar ratio of-OH groups in the component A to-NCO groups in the component B, namely mixing 53 parts of the component A with 47 parts of the component B, stirring and mixing for 30s at the rotating speed of 2200rpm, then placing the mixture in a vacuum condition of less than or equal to 0.09MPa for vacuum defoaming for 8min, then placing the mixture into a mold preheated to 75 ℃, then placing the mold into a 75 ℃ oven for curing for 1h, and then curing for 50h at 28 ℃ to obtain the non-foaming polyurethane elastomer with excellent mechanical properties.
The prepared unfoamed polyurethane elastomer is subjected to microscopic morphology characterization, and no obvious cell defect in the prepared polyurethane elastomer can be observed, which indicates that the defoaming is complete in the preparation process. The tensile strength and elongation at break of the non-foamed polyurethane elastomer prepared were tested with reference to the standard GB/T1040.3-2006, and the tensile strength of the polyurethane elastomer was 18.68MPa and the elongation at break was 745%.
Comparative example 1
(1) Respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, the PTMEG 330N and the BDO until the water content is less than or equal to 500 ppm;
(2) uniformly mixing 70.9 parts of dehydrated PTMEG2000, 19.7 parts of 330N, 0.1 part of T-12, 7.4 parts of dehydrated BDO and 1.9 parts of X-313 (a defoaming agent of New Material company, Guangzhou, Detian, with the model number of X-313) to obtain a component A;
uniformly mixing 45 parts of MDI and 55 parts of PTMEG under the nitrogen protection atmosphere, and stirring and reacting for 4 hours at 80-85 ℃ to obtain a prepolymer capped by-NCO, which is abbreviated as a component B and has the NCO content of 12.9%;
(3) respectively preheating the component A and the component B to 30 ℃, then mixing the preheated component A and the preheated component B according to the molar ratio of-OH groups in the component A to-NCO groups in the component B of 1.05, stirring and mixing for 30s at the rotating speed of 2000rpm, then placing the mixture in a vacuum degree of less than or equal to 0.09MPa for 10min, then placing the mixture in a mold preheated to 70 ℃, then placing the mold in a 70 ℃ oven for curing for 1.5h, and then curing for 48h at 25 ℃ to obtain the non-foaming polyurethane elastomer.
The micro-morphology characterization of the prepared non-foamed polyurethane elastomer is carried out, and as can be seen from the SEM picture in FIG. 2, obvious cells exist in the polyurethane elastomer, which indicates that the defoaming is incomplete in the preparation process. The tensile strength and elongation at break of the non-foamed polyurethane elastomer prepared were tested with reference to the standard GB/T1040.3-2006, and the tensile strength and elongation at break of the polyurethane elastomer were measured to be 11.76MPa and 484%.
Comparative example 2
(1) Respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, the PTMEG 330N and the BDO until the water content is less than or equal to 500 ppm;
(2) dissolving 0.02 part of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; uniformly mixing 70.9 parts of dehydrated PTMEG2000, 19.7 parts of 330N containing T-12, 7.4 parts of dehydrated BDO and 1.9 parts of X-313 (a defoaming agent of a New Material company, Guangzhou, No. X-313) to obtain a component A;
uniformly mixing 45 parts of MDI and 55 parts of PTMEG under the nitrogen protection atmosphere, and stirring and reacting for 4 hours at 80-85 ℃ to obtain a prepolymer capped by-NCO, which is abbreviated as a component B and has an NCO content of 12.6%;
(3) respectively preheating the component A and the component B to 30 ℃, then mixing the preheated component A and the component B according to the molar ratio of-OH groups in the component A to-NCO groups in the component B of 1.05, stirring and mixing at the rotating speed of 1700rpm for 16s, then placing the mixture in a vacuum degree of less than or equal to 0.09MPa for vacuum defoaming for 7min, then placing the mixture in a mold preheated to 65 ℃, then placing the mold in a 70 ℃ oven for curing for 1.5h, and then curing for 48h at 18 ℃ to obtain the non-foaming polyurethane elastomer.
The micro-morphology characterization of the prepared non-foamed polyurethane elastomer is carried out, and as can be seen from the SEM picture in FIG. 3, obvious cells exist in the polyurethane elastomer, which indicates that the defoaming is incomplete in the preparation process. The tensile strength and elongation at break of the non-foamed polyurethane elastomer prepared were tested with reference to the standard GB/T1040.3-2006, and the tensile strength of the polyurethane elastomer was 15.25MPa and the elongation at break was 602%.
According to the mechanical properties of the polyurethane elastomers prepared in the embodiments 1-2 and the comparative examples 1-2, the content of the catalyst is regulated and the process parameters of the preparation process are optimized, so that bubbles introduced in the preparation process can be effectively removed through defoaming, the defect of a bubble hole in a product is reduced, and the tensile strength and the elongation at break of the polyurethane elastomer are obviously improved.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of a non-foaming polyurethane elastomer with excellent mechanical properties is characterized by comprising the following steps: the method comprises the following steps:
stirring and mixing the component A and the component B which are preheated to (30 +/-2) ° C for (25 +/-5) s at the rotating speed of 1900-2200 rpm, then placing the mixture in a vacuum degree condition of less than or equal to 0.09MPa for vacuum defoamation for 8 min-10 min, then placing the mixture in a mold preheated to (75 +/-5) ° C, then placing the mold in a (75 +/-5) ° C oven for curing for 1 h-1.5 h, and then curing the mold at (25 +/-5) ° C for (48 +/-5) h to obtain a non-foaming polyurethane elastomer with excellent mechanical property;
the component A is prepared by mixing PTMEG2000, 330N, BDO, X-313 and T-12; wherein the component A comprises the following components in parts by weight: PTMEG 200070-71 parts, 330N 19-20 parts, BDO 7.3-7.5 parts, X-3131.8-2.0 parts and T-120.0003-0.002 parts;
the component B is a prepolymer with NCO content of 12-13 percent formed by the reaction of isocyanate containing-NCO groups and PTMEG 2000;
wherein the molar ratio of-OH groups in the component A to-NCO groups in the component B is (1.03-1.07): 1; the water content of PTMEG2000, 330N and BDO is less than or equal to 500 ppm.
2. The method for preparing a non-foaming polyurethane elastomer with excellent mechanical properties as claimed in claim 1, wherein the method comprises the following steps: the component B is a prepolymer with NCO content of 12-13% formed by stirring and reacting isocyanate containing-NCO groups and PTMEG2000 at 80-85 ℃ for 3.8-4.2 h.
3. The method for preparing a non-foaming polyurethane elastomer with excellent mechanical properties according to claim 1 or 2, wherein: the isocyanate containing-NCO groups is MDI.
4. The method for preparing a non-foaming polyurethane elastomer with excellent mechanical properties as claimed in claim 3, wherein: the component B comprises the following components in parts by weight: PTMEG 200054-57 parts and MDI 44-47 parts.
5. The method for preparing a non-foaming polyurethane elastomer with excellent mechanical properties as claimed in claim 1, wherein the method comprises the following steps: t-12 was dissolved in 330N and mixed with PTMEG2000, BDO and X-313.
6. The method for preparing a non-foaming polyurethane elastomer with excellent mechanical properties as claimed in claim 1, wherein the method comprises the following steps: the weight portion of T-12 in the component A is 0.0003-0.0005.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020055604A1 (en) * | 2000-06-14 | 2002-05-09 | Freeland Gerard Scott | Liquid stable MDI prepolymers and liquid stable curative systems suitable for room temperature casting which yield high performance urethane elastomers |
| US20050033007A1 (en) * | 2002-03-07 | 2005-02-10 | Asahi Glass Company Limited | Thermosetting polyurethane elastomer composition, polyurethane elastomer and method for its production |
| CN105461877A (en) * | 2015-12-21 | 2016-04-06 | 中国科学院山西煤炭化学研究所 | Synthetic method of thermocuring polyurethane elastomer composite material for sealing materials |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020055604A1 (en) * | 2000-06-14 | 2002-05-09 | Freeland Gerard Scott | Liquid stable MDI prepolymers and liquid stable curative systems suitable for room temperature casting which yield high performance urethane elastomers |
| US20050033007A1 (en) * | 2002-03-07 | 2005-02-10 | Asahi Glass Company Limited | Thermosetting polyurethane elastomer composition, polyurethane elastomer and method for its production |
| CN105461877A (en) * | 2015-12-21 | 2016-04-06 | 中国科学院山西煤炭化学研究所 | Synthetic method of thermocuring polyurethane elastomer composite material for sealing materials |
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| Title |
|---|
| 山西省化工研究所编: "《聚氨酯弹性体手册》", 31 January 2001, 化学工业出版社 * |
| 王台: "光学微流变法研究室温浇注聚氨酯固化体系的反应特性", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 罗建勋等: "混合扩链剂对聚氨酯弹性体宏观性能的影响", 《北京化工大学学报(自然科学版)》 * |
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