CN119684775A - Waterborne polyurethane conductive sponge and preparation method and application thereof - Google Patents
Waterborne polyurethane conductive sponge and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a waterborne polyurethane conductive sponge and a preparation method and application thereof, belonging to the technical field of conductive sponge, wherein the waterborne polyurethane conductive sponge comprises the following components in parts by weight: 26-30 parts of aqueous polyurethane emulsion, 6-8 parts of soluble modified carbon black, 3-5 parts of mesoporous titanium oxide, 0.5-1 part of dispersing agent, 2-3 parts of foaming agent and 78-82 parts of water. The invention ensures that the prepared conductive sponge has excellent mechanical property and conductivity.
Description
Technical Field
The invention belongs to the technical field of conductive sponge, and particularly relates to a waterborne polyurethane conductive sponge, and a preparation method and application thereof.
Background
The conductive sponge is a three-dimensional porous net structural material, and has the characteristics of heat preservation, heat insulation, sound absorption, shock absorption, flame retardance, static resistance, good air permeability, good conductivity and the like, so that the conductive sponge is widely applied to various electronic and mobile communication equipment and is popular with the masses.
The existing conductive sponge is generally prepared by adding carbon black into aqueous polyurethane emulsion so as to improve the conductivity of the conductive sponge. Carbon black, while capable of enhancing the conductivity of conductive sponges, also has some drawbacks.
Carbon black has a high specific surface area and adsorption properties, and carbon black particles are poor in dispersibility and easy to agglomerate, so that the carbon black is unevenly dispersed in a polymer matrix. The agglomerated carbon black particles form stress concentration points in the conductive sponge, thereby reducing the overall strength of the conductive sponge, i.e., affecting the mechanical properties of the conductive sponge. The non-uniformity of the carbon black particle distribution also results in a sponge having a relatively high volume resistivity, i.e., affecting the conductive properties of the conductive sponge.
Disclosure of Invention
In order to solve the problems in the background technology, the invention provides a waterborne polyurethane conductive sponge, a preparation method and application thereof, and the prepared conductive sponge is ensured to have excellent mechanical property and conductivity.
In order to achieve the aim, the invention provides an aqueous polyurethane conductive sponge which comprises, by weight, 26-30 parts of aqueous polyurethane emulsion, 6-8 parts of soluble modified carbon black, 3-5 parts of mesoporous titanium oxide, 0.5-1 part of a dispersing agent, 2-3 parts of a foaming agent and 78-82 parts of water.
Further, the preparation method of the mesoporous titanium oxide comprises the following steps:
a1, slowly adding butyl titanate and acetylacetone into an ethanol water solution containing cetyltrimethylammonium bromide at the same time, and stirring for 1h at room temperature to obtain a first solution;
a2, adding concentrated hydrochloric acid into the ethanol water solution, and uniformly mixing to obtain a second solution;
a3, adding the second solution obtained in the step A2 into the first solution obtained in the step A1 at a dropping speed of 1-2 drops/s, and continuously stirring for 4 hours to obtain a sol solution with a pH value of 3-4, wherein the molar ratio of butyl titanate, acetylacetone, cetyltrimethylammonium bromide, ethanol and water is 1:0.3:0.05 (14-18): 5;
And A4, after the sol solution obtained in the step A3 is gelled for 12 hours, aging, drying and roasting are sequentially carried out, and thus the mesoporous titanium oxide is obtained.
Further, in A4, the specific operation of aging is that the mixture is aged for 1d at a temperature of 20-25 ℃ and then aged for 2-3d at a temperature of 65-75 ℃.
Further, in A4, the specific operation of drying is that the temperature is raised to 110-120 ℃ at the speed of 2 ℃ per minute, and the temperature is kept for 10-12 hours.
Further, in A4, the specific operation of roasting is that the temperature is raised to 340-350 ℃ at the speed of 1 ℃ per minute, and the temperature is kept for 4-5 hours.
Further, the preparation method of the soluble modified carbon black comprises the following steps:
B1, 5g of carbon black and 150mL of nitric acid with the mass fraction of 67% are taken and placed in a three-mouth bottle, and reacted for 72-80h at 100 ℃ under the stirring condition to obtain a first reactant;
b2, centrifugally separating the first reactant to obtain a soluble substance and a first insoluble substance, concentrating the soluble substance by using a rotary evaporator, and continuously adding water for washing after concentrating until the PH value of the eluent is 7 to obtain a first solution;
B3, washing the first insoluble matters with water, centrifugally separating the washing liquid into a second solution and a second insoluble matters, continuously washing the second insoluble matters with water, centrifugally separating the washing liquid into a third solution and a third insoluble matters, combining the third solution, the second solution and the first solution, concentrating by using a rotary evaporator to obtain a concentrated solution, and drying at 120-130 ℃ for 8-10h to obtain the soluble modified carbon black.
Further, the dispersant comprises a polysilicone dispersant and/or a polyether silicone dispersant.
Further, the foaming agent comprises coconut oil fatty acid diethanolamide and/or sodium dodecyl polyoxyethylene ether sulfate.
The second aspect of the invention provides a preparation method of the aqueous polyurethane conductive sponge, which comprises the following steps of diluting aqueous polyurethane emulsion with water, adding a dispersing agent, soluble modified carbon black and mesoporous titanium oxide, stirring for 10-15min, adding a foaming agent, stirring for 15-20min, then placing in a 60-80 ℃ blowing oven for curing and forming, and finally placing for 20-24h under the condition of room temperature ventilation to obtain the aqueous polyurethane conductive sponge.
In a third aspect, the invention provides an application of the aqueous polyurethane conductive sponge, which is used for electronic products, medical devices and packaging materials.
The application has the following beneficial effects:
1. mesoporous titanium oxide has a unique pore structure and a large specific surface area, and the soluble modified carbon black provides more attachment points and reaction sites. When the soluble modified carbon black is combined with the mesoporous titanium oxide, the soluble modified carbon black is uniformly distributed on the surface and in the pores of the mesoporous titanium oxide to form a more complex network structure, and the structure not only increases the specific surface area of the conductive sponge, but also improves the mechanical property of the conductive sponge. When the soluble modified carbon black is filled into the pores of the mesoporous titanium oxide, the composite structure formed by the soluble modified carbon black and the mesoporous titanium oxide has more optimized pore distribution situation and mechanical property, and is beneficial to improving the conductivity and mechanical property of the conductive sponge.
2. The oxygen-containing functional groups are introduced into the surface of the soluble modified carbon black, the functional groups have higher chemical activity and react with active sites on the surface of the mesoporous titanium oxide to form stable chemical bonds, the bonding force between the soluble modified carbon black and the mesoporous titanium oxide is enhanced, the mechanical property of the conductive sponge is improved, when the mesoporous titanium oxide is combined with the soluble modified carbon black, the pore channel structure of the mesoporous titanium oxide is favorable for the dispersion and uniform distribution of the soluble modified carbon black, so that the formation of a conductive network is optimized, a more optimized conductive network is formed in the conductive sponge, the conductive network not only improves the conductivity of the conductive sponge, but also promotes the transmission of electrons in the conductive network, and in the conductive network, the electron transmission speed between the soluble modified carbon black and the mesoporous titanium oxide is obviously improved because the oxygen-containing functional groups on the surface of the soluble modified carbon black serve as a 'springboard' of electrons, and the jumping type transmission of electrons among the mesoporous titanium oxide is promoted, and the electronic transmission mechanism can further improve the conductivity of the conductive sponge.
Drawings
Fig. 1, comparative trend graphs of mechanical properties (tensile strength) test data of conductive sponges prepared in examples 1 to 4 of the present invention and comparative examples 1 to 5;
fig. 2, comparative trend graphs of the conductive properties (volume resistivity) test data of the conductive sponges prepared in examples 1 to 4 of the present invention and comparative examples 1 to 5.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials of the examples and comparative examples of the present application are commercially available in general except for the specific descriptions.
Example 1 (1) the method for preparing mesoporous titanium oxide is as follows:
a1, 2mol of butyl titanate and 0.6mol of acetylacetone are simultaneously slowly added to an ethanol aqueous solution containing 0.1mol of cetyltrimethylammonium bromide, wherein the ethanol aqueous solution comprises 24mol of ethanol and 8mol of water. Stirring at a constant speed of 180r/min for 1h at room temperature to obtain a first solution.
A2, adding concentrated hydrochloric acid into an ethanol aqueous solution, wherein the ethanol aqueous solution comprises 6mol of ethanol and 2mol of water, stirring at a constant speed of 180r/min for 5min, and uniformly mixing to obtain a second solution.
A3, adding the second solution obtained in the step A2 into the first solution obtained in the step A1 at a dropping speed of 1 drop/s, and continuously stirring at a constant speed of 180r/min for 4 hours to obtain a sol solution, wherein the pH value of the sol solution is 3.5.
A4, placing and gelling the sol solution obtained in the step A3 for 12 hours, and sequentially aging, drying and roasting, wherein the specific operation of aging is that the sol solution is aged for 1d at the temperature of 22 ℃ and then aged for 2d at the temperature of 70 ℃, the specific operation of drying is that the sol solution is heated to 115 ℃ at the speed of 2 ℃ per minute and is kept for 12 hours, the specific operation of roasting is that the sol solution is continuously heated to 345 ℃ at the speed of 1 ℃ per minute and is kept for 5 hours, and the mesoporous titanium oxide is obtained.
Wherein, butyl titanate (99%) is purchased from Shandong Linguan fine chemical industry Co., ltd. Acetylacetone (technical grade 99.5%) was purchased from shandong signal chemostat company, inc. Cetyl trimethylammonium bromide (99%) was purchased from Anhui Ponhao chemical Co.
(2) The preparation method of the soluble modified carbon black comprises the following steps:
B1, 5g of carbon black and 150mL of nitric acid with the mass fraction of 67% are taken and placed in a three-mouth bottle, and reacted for 75 hours at 100 ℃ under the stirring condition at the speed of 150r/min to obtain a first reactant.
And B2, centrifugally separating the first reactant to obtain a soluble substance and a first insoluble substance, concentrating the soluble substance by using a rotary evaporator, and then continuously adding water for washing until the PH value of the eluent is 7, thus obtaining a first solution.
B3, washing the first insoluble matters with water, centrifugally separating the washing liquid into a second solution and a second insoluble matters, continuously washing the second insoluble matters with water, centrifugally separating the washing liquid into a third solution and a third insoluble matters, combining the third solution, the second solution and the first solution, concentrating by using a rotary evaporator to obtain a concentrated solution, and drying at 125 ℃ for 9 hours to obtain the soluble modified carbon black.
Wherein, carbon black (VXC-72) is purchased from Tianjin, tianji chemical industry product technology development Co.
(3) A preparation method of the waterborne polyurethane conductive sponge comprises the following steps of firstly diluting 28 parts of waterborne polyurethane emulsion with 80 parts of water according to parts by weight, specifically operating the steps of adding the 28 parts of waterborne polyurethane emulsion into the 80 parts of water, stirring at a constant speed of 220r/min for 20min to uniformly mix, then adding 0.8 part of dispersing agent, 7 parts of soluble modified carbon black and 4 parts of mesoporous titanium oxide, continuously stirring at a constant speed of 220r/min for 13min, adding 2.5 parts of foaming agent, continuously stirring at a constant speed of 220r/min for 17min, then placing in a 70 ℃ blast oven for 24h, curing and forming, and finally placing for 22h under a room temperature ventilation condition to obtain the waterborne polyurethane conductive sponge.
Wherein the aqueous polyurethane emulsion (Basoff, ECO 3702) is purchased from Nanhai Heng Xiuhui chemical Co., ltd. The dispersant is BYK polyether organosilicon copolymer dispersant purchased from Xin Ying trade Limited company in Guangzhou city. The foaming agent is coconut oil fatty acid diethanolamide, which is purchased from Guangzhou City chemical industry Co.
The embodiment 2 is different from the embodiment 1 in that (3) a preparation method of the waterborne polyurethane conductive sponge comprises the following steps of diluting 26 parts of waterborne polyurethane emulsion with 78 parts of water, adding 0.5 part of dispersing agent, 6 parts of soluble modified carbon black and 3 parts of mesoporous titanium oxide, stirring for 10min, adding 2 parts of foaming agent, stirring for 15min, then placing in a 60 ℃ blowing oven for curing and forming, and finally placing for 20h under the condition of room temperature ventilation to obtain the waterborne polyurethane conductive sponge.
The embodiment 3 is different from the embodiment 1 in that (3) the preparation method of the aqueous polyurethane conductive sponge comprises the following steps of diluting 30 parts of aqueous polyurethane emulsion with 82 parts of water, adding 1 part of dispersing agent, 8 parts of soluble modified carbon black and 5 parts of mesoporous titanium oxide, stirring for 15min, adding 3 parts of foaming agent, stirring for 20min, then placing in an 80 ℃ blowing oven for curing and forming, and finally placing for 24h under the condition of room temperature ventilation to obtain the aqueous polyurethane conductive sponge.
The embodiment 4 is different from the embodiment 1 in that (3) the preparation method of the waterborne polyurethane conductive sponge comprises the following steps of diluting 30 parts of waterborne polyurethane emulsion with 78 parts of water, adding 0.6 part of dispersing agent, 7 parts of soluble modified carbon black and 4 parts of mesoporous titanium oxide, stirring for 12min, adding 2.5 parts of foaming agent, stirring for 15min, then placing in a 75 ℃ blowing oven for curing and forming, and finally placing for 22h under the condition of room temperature ventilation to obtain the waterborne polyurethane conductive sponge.
Comparative example 1 this comparative example differs from example 1 in that mesoporous titanium oxide was deleted and the soluble modified carbon black was replaced with carbon black.
The preparation method comprises the following steps of diluting 28 parts of aqueous polyurethane emulsion with 80 parts of water according to parts by weight, adding 0.8 part of dispersing agent and 7 parts of carbon black, stirring at a constant speed of 220r/min for 13min, adding 2.5 parts of foaming agent, continuously stirring at a constant speed of 220r/min for 17min, placing in a 70 ℃ blast oven for 24h, curing and forming, and finally placing for 22h under a room temperature ventilation condition to obtain the aqueous polyurethane conductive sponge.
Comparative example 2 this comparative example differs from example 1 in that the mesoporous titanium oxide was replaced with titanium oxide and the soluble modified carbon black was replaced with carbon black.
The preparation method comprises the steps of diluting 28 parts of aqueous polyurethane emulsion with 80 parts of water according to parts by weight, adding 0.8 part of dispersing agent, 7 parts of carbon black and 4 parts of titanium oxide, continuously stirring at a constant speed of 220r/min for 13min, adding 2.5 parts of foaming agent, continuously stirring at a constant speed of 220r/min for 17min, then placing in a 70 ℃ blast oven for 24h, curing and forming, and finally placing for 22h under a room temperature ventilation condition to obtain the aqueous polyurethane conductive sponge. Wherein the titanium oxide is purchased from Handersen chemical Co., ltd.
Comparative example 3 this comparative example differs from example 1 in that the soluble modified carbon black was replaced with carbon black.
The preparation method comprises the steps of diluting 28 parts of aqueous polyurethane emulsion with 80 parts of water according to parts by weight, adding 0.8 part of dispersing agent, 7 parts of carbon black and 4 parts of mesoporous titanium oxide, continuously stirring at a constant speed of 220r/min for 13min, adding 2.5 parts of foaming agent, continuously stirring at a constant speed of 220r/min for 17min, then placing in a 70 ℃ blast oven for 24h, curing and forming, and finally placing for 22h under the condition of room temperature ventilation to obtain the aqueous polyurethane conductive sponge.
Comparative example 4 this comparative example differs from example 1 in that the mesoporous titania was replaced with titania.
The preparation method comprises the following steps of firstly diluting 28 parts of aqueous polyurethane emulsion with 80 parts of water according to parts by weight, then adding 0.8 part of dispersing agent, 7 parts of soluble modified carbon black and 4 parts of titanium oxide, continuously stirring at a constant speed of 220r/min for 13min, then adding 2.5 parts of foaming agent, continuously stirring at a constant speed of 220r/min for 17min, then placing in a 70 ℃ blast oven for 24h, curing and forming, and finally placing for 22h under the condition of room temperature ventilation to obtain the aqueous polyurethane conductive sponge.
Comparative example 5 this comparative example differs from example 1 in that the soluble modified carbon black was replaced with an insoluble modified carbon black.
The preparation method comprises the following steps of firstly diluting 28 parts of aqueous polyurethane emulsion with 80 parts of water according to parts by weight, then adding 0.8 part of dispersing agent, 7 parts of insoluble modified carbon black and 4 parts of mesoporous titanium oxide, continuously stirring at a constant speed of 220r/min for 13min, then adding 2.5 parts of foaming agent, continuously stirring at a constant speed of 220r/min for 17min, then placing in a 70 ℃ blast oven for 24h, curing and forming, and finally placing for 22h under a room temperature ventilation condition to obtain the aqueous polyurethane conductive sponge.
The insoluble modified carbon black is prepared by the following steps:
B1, 5g of carbon black and 150mL of nitric acid with the mass fraction of 67% are taken and placed in a three-mouth bottle, and reacted for 75 hours at 100 ℃ under the stirring condition at the speed of 150r/min to obtain a first reactant.
And B2, centrifugally separating the first reactant to obtain a soluble substance and an insoluble substance, washing the insoluble substance with water until the PH value of a washing solution is 7, and then drying the insoluble substance washed to be neutral at 125 ℃ for 9 hours to obtain the insoluble modified carbon black.
Test example the test subjects were conductive sponges prepared in examples 1 to 4 and comparative examples 1 to 5. The mechanical properties (tensile strength) and electrical conductivity (volume resistivity) of each test object (conductive sponge) are shown in table 1.
TABLE 1 test example test data
| Tensile Strength/MPa | Volume resistivity/. Times.10 10 4 Ω & cm | |
| Example 1 | 0.078 | 2.35 |
| Example 2 | 0.075 | 2.36 |
| Example 3 | 0.081 | 2.34 |
| Example 4 | 0.077 | 2.34 |
| Comparative example 1 | 0.060 | 3.87 |
| Comparative example 2 | 0.061 | 3.86 |
| Comparative example 3 | 0.067 | 3.45 |
| Comparative example 4 | 0.058 | 4.12 |
| Comparative example 5 | 0.072 | 2.75 |
As can be seen from the analysis of the data of the examples 1-4 and the combination of the data of the table 1 and the data of the figures 1-2, the conductive sponge prepared by the invention has excellent mechanical property and conductivity, the tensile strength reaches more than 0.075MPa, and the volume resistivity is as low as below 2.36 x 10 4 omega cm.
As can be seen from the analysis of the data of examples 1 and 1-5 and the comparison of fig. 1-2, the addition of titanium oxide to the raw material composition of comparative example 1 and comparative example 2, compared with comparative example 1, resulted in the tensile strength test data of comparative example 2 of 0.062MPa, slightly greater than 0.060MPa of comparative example 1, and the volume resistivity test data of comparative example 2 of 3.86 x 10 4 Ω cm, slightly lower than 3.87 x 10 4 Ω cm of comparative example 1. The addition of titanium oxide has little influence on the tensile strength and volume resistivity of the prepared conductive sponge.
As can be seen from comparison of comparative examples 1 and 3, the addition of mesoporous titanium oxide to the raw material composition of comparative example 3 resulted in comparative example 3 having a tensile strength test data of 0.067MPa, which is significantly greater than that of comparative example 1, and comparative example 3 having a volume resistivity test data of 3.45×10 4 Ω·cm, which is significantly less than that of comparative example 1. The addition of mesoporous titanium oxide can improve the tensile strength of the prepared conductive sponge, reduce the volume resistivity of the prepared conductive sponge, and improve the mechanical property and the conductivity of the prepared conductive sponge.
As can be seen from comparison of comparative examples 2 and 4, comparative example 4, in which the carbon black in the raw material component was replaced with the soluble modified carbon black, compared with comparative example 2 (the raw material component contained carbon black and titanium oxide), resulted in that the tensile strength test data of the conductive sponge prepared in comparative example 4 was 0.058MPa, which is less than 0.062MPa of comparative example 2, and the volume resistivity test data of the conductive sponge prepared in comparative example 4 was 4.12× 4 Ω·cm, which is greater than 3.86× 4 Ω·cm of comparative example 2. When titanium oxide exists in the raw material components, the carbon black in the raw material components is replaced by soluble modified carbon black, but the tensile strength of the prepared conductive sponge is reduced, the volume resistivity is increased, and the mechanical property and the conductivity of the prepared conductive sponge are reduced.
This is because, compared to carbon black, the solubility of the soluble modified carbon black is increased, so that the solubility is too high, which results in excessive dispersion or aggregation in the matrix, thereby affecting the uniform distribution thereof in the matrix, while the adsorption capacity of titanium oxide is limited and lacks selectivity, and the inability to provide stable, reliable and uniform adsorption to the soluble modified carbon black results in insufficient bonding strength and failure to form a stable, reliable and uniform-texture conductive network, which ultimately results in a decrease in the mechanical properties and conductive properties of the resulting conductive sponge.
As is clear from comparison of comparative examples 3 and 5, comparative example 5, in which the carbon black in the raw material component was replaced with the insoluble modified carbon black, compared with comparative example 3 (the raw material component contained carbon black and mesoporous titanium oxide), resulted in that the tensile strength test data of the conductive sponge prepared in comparative example 5 was 0.072MPa, which was greater than 0.067MPa of comparative example 3, and the volume resistivity test data of the conductive sponge prepared in comparative example 5 was 2.75×10 4 Ω·cm, which was less than 3.45×10 4 Ω·cm of comparative example 3. When the mesoporous titanium oxide is present in the raw material components, the carbon black in the raw material components is replaced by insoluble modified carbon black, so that the tensile strength of the prepared conductive sponge can be improved, the volume resistivity of the prepared conductive sponge can be reduced, and the mechanical property and the conductivity of the prepared conductive sponge are improved.
As is clear from comparison of comparative example 3 and example 1, in example 1, the carbon black in the raw material component was replaced with the soluble modified carbon black, and as a result, the tensile strength test data of the conductive sponge prepared in example 1 was 0.078MPa, which is significantly greater than that of comparative example 3, and the volume resistivity test data of the conductive sponge prepared in example 1 was 2.35×10 4 Ω·cm, which is significantly less than that of comparative example 3, which is 3.45×10 4 Ω·cm. When the mesoporous titanium oxide is present in the raw material components, the carbon black in the raw material components is replaced by soluble modified carbon black, so that the tensile strength of the prepared conductive sponge can be improved, the volume resistivity of the prepared conductive sponge can be reduced, and the mechanical property and the conductivity of the prepared conductive sponge can be improved.
In summary, when titanium oxide is used as the raw material component, the carbon black is replaced by soluble modified carbon black, which can lead to the decrease of the mechanical property and the conductivity of the prepared conductive sponge. When the mesoporous titanium oxide is used as the raw material component, the carbon black is replaced by insoluble modified carbon black, so that the mechanical property and the conductivity of the prepared conductive sponge can be improved, and when the carbon black is replaced by soluble modified carbon black, the mechanical property and the conductivity of the prepared conductive sponge can be further improved. The method shows that the mesoporous titanium oxide and the soluble modified carbon black have a synergistic effect, and the mechanical property and the conductivity of the prepared conductive sponge can be synergistically improved.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
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Denomination of invention: A water-based polyurethane conductive sponge and its preparation method and application Granted publication date: 20250610 Pledgee: Bank of China Limited Yongxiu sub branch Pledgor: Jiangxi boyihong Electronics Co.,Ltd. Registration number: Y2025980056192 |