CN109337149B - Multifunctional rubber composite material containing bacterial cellulose and preparation method thereof - Google Patents
Multifunctional rubber composite material containing bacterial cellulose and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multifunctional rubber composite material containing bacterial cellulose and a preparation method thereof.A complete bacterial cellulose three-dimensional network structure is reconstructed in a polyvinyl alcohol/rubber composite material by adopting a dissolving-regenerating process, so that the bacterial cellulose in the three-dimensional network structure can well reinforce the composite material on one hand, and the water response characteristic of the composite material is realized by utilizing the hydrogen bond effect in the three-dimensional network on the other hand; the polyvinyl alcohol in the composite material plays a role of a compatilizer and plastic, avoids the heat vulcanization of rubber, and obtains the water-responsive functional rubber composite material with good recovery effect.
Description
Technical Field
The invention belongs to the technical field of preparation of functional rubber, and particularly relates to a multifunctional rubber composite material containing bacterial cellulose and a preparation method thereof.
Background
The functional material is a material system which can judge, process and react on the information about environmental conditions and changes acquired from the surface layer or the inside of the material system to change the structure and the function of the material system so as to be well coordinated with the outside and has self-adaptability. Rubber is a material with high elasticity, and is widely applied to various fields of national economy. The intellectualization of rubber materials has been a research hotspot in the rubber industry.
The functional rubber is prepared by synthesizing rubber with a novel molecular chain structure or adding functional fillers to endow the traditional rubber material with new functions. The former involves special monomers and new synthesis processes, and is too high in cost and difficult to realize industrialization. The latter mainly realizes the functionalization of rubber materials at lower cost through the selection of functional fillers and the design of a forming process, and is widely concerned by researchers. Bacterial Cellulose (BC) is a novel high molecular compound, is synthesized by microorganisms such as acetobacter xylinum, agrobacterium tumefaciens and rhizobium, has a three-dimensional network structure in a microstructure, has the characteristics of high chemical purity, high crystallinity, good biocompatibility, strong water absorption capacity, high mechanical strength, biodegradability and the like, and is a potential functional filler. If the microscopic three-dimensional network structure of the bacterial cellulose is kept in the rubber, the function of the bacterial cellulose is important to be exerted.
Disclosure of Invention
The invention aims to provide a multifunctional rubber composite material containing bacterial cellulose and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows:
the multifunctional rubber composite material containing the bacterial cellulose is prepared from 30-70 parts by mass of the bacterial cellulose, 100 parts by mass of rubber and 30-50 parts by mass of polyvinyl alcohol.
The size of the bacterial cellulose is 1000-2000 meshes.
The rubber is any one of styrene butadiene rubber, natural rubber or nitrile butadiene rubber.
The polyvinyl alcohol has the molecular weight of 5000-10000 and the alcoholysis degree of 90-98%.
A preparation method of a multifunctional rubber composite material containing bacterial cellulose comprises the following steps:
the method comprises the following steps: preparing a mixed solution of 5-10wt% of sodium hydroxide and 7-15wt% of urea, adding 30-70 parts of bacterial cellulose, and performing ultrasonic dispersion uniformly to obtain a bacterial cellulose solution;
step two: adding 5-20 parts by mass of polyvinyl alcohol into water, heating and stirring to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and uniformly dispersing by ultrasonic to obtain a polyvinyl alcohol modified bacterial cellulose water dispersion solution;
step three: adding 25-45 parts by mass of polyvinyl alcohol into water, heating and stirring to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, uniformly dispersing by ultrasonic, adding the polyvinyl alcohol modified bacterial cellulose aqueous dispersion obtained in the step two, continuously dispersing by ultrasonic, carrying out spray drying on the obtained mixed solution to obtain rubber powder, and carrying out hot pressing on the powder at the temperature of 130-140 ℃ and the pressure of 0.5-1.5MPa for 10-20min to obtain the multifunctional rubber composite material containing the bacterial cellulose.
Further, in the first step, ultrasonic treatment is carried out for 0.5-1h at 500- & lt 1000 & gtW.
Further, in the second step, heating to 95 ℃ and stirring for 1-3h to obtain the polyvinyl alcohol solution.
Further, in the second step, ultrasound is performed for 0.5-1h at 500- & lt1000 & gtW.
Further, in the third step, heating to 95 ℃, and stirring for 1-3h to obtain the polyvinyl alcohol solution.
Further, in the third step, ultrasonic treatment is performed for 1-2 hours under the conditions of 500 + 1000W.
Further, in the third step, ultrasonic dispersion is continued for 0.5 to 1 hour.
Compared with the prior art, the invention has the following remarkable advantages:
(1) through a three-component composite system of bacterial cellulose/polyvinyl alcohol/rubber, on one hand, the plastic phase effect of the polyvinyl alcohol is utilized to blend the polyvinyl alcohol and the rubber, so that the vulcanization crosslinking process of the rubber is avoided, and the rubber has heat recoverability; on the other hand, the compatibility of polyvinyl alcohol is utilized to transfer external stress between rubber and bacterial cellulose;
(2) the three-dimensional network structure of the bacterial cellulose is reconstructed in the rubber composite material by utilizing a dissolving-regenerating process, so that the composite material can bear larger external stress and the reinforcement of the composite material is realized; on the other hand, the three-dimensional hydrogen bond network rich in bacterial cellulose is utilized, the correspondence of an external water adding environment is realized, and the water responsiveness function is realized.
Drawings
FIG. 1 is a schematic flow chart of the method for preparing the rubber composite material containing bacterial cellulose according to the present invention.
Fig. 2 is an SEM photograph of bacterial cellulose.
Detailed Description
The present invention is further illustrated by the following examples and comparative examples.
Referring to fig. 1, the preparation method of the multifunctional rubber composite material containing bacterial cellulose of the present invention comprises the following steps:
the method comprises the following steps: preparing 300mL of 5-10wt% sodium hydroxide/7-15 wt% urea mixed solution, adding 30-70 parts of bacterial cellulose with the size of 1000-;
step two: adding 5-20 parts by mass of polyvinyl alcohol with the molecular weight of 5000-10000 and the alcoholysis degree of 90-98% into 500mL of deionized water, heating to 95 ℃, stirring for 1-3h to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing 500-1000W ultrasonic treatment for 0.5-1h to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 25-45 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 1-3h to obtain a polyvinyl alcohol solution, mixing with rubber latex, wherein the rubber latex is any one of styrene butadiene rubber, natural rubber or nitrile butadiene rubber, the corresponding dry rubber amount is 100 parts by mass, carrying out ultrasonic treatment at 500- > 1000W for 1-2h, adding the aqueous dispersion obtained in the step two, continuing ultrasonic treatment for 0.5-1h, carrying out spray drying on the obtained mixed solution to obtain rubber powder, and carrying out hot pressing on the powder at 130- > 140 ℃ and 0.5-1.5MPa for 10-20min to obtain the multifunctional rubber composite material containing the bacterial cellulose.
The obtained rubber composite was subjected to the following performance tests
(1) Hardness of
The hardness of the test specimens was determined according to GB/T531-1999 using an LX-A rubber hardness tester from nine instruments, Inc., Shanghai.
(2) Tensile Properties
According to GB/T528-.
(3) Tear performance
According to GB/T529-.
(4) Water response performance
Cutting the rubber composite material into a wafer with the diameter of 75mm and the thickness of 2mm, soaking the wafer in 500mL of deionized water for 24 hours, and measuring the change degree of the diameter of the wafer, wherein the calculation mode of the change degree of the diameter is as follows: the diameter variation (diameter after soaking-diameter before soaking)/diameter before soaking; drying the soaked sample, cutting the sample into tensile samples, re-measuring the tensile strength, and calculating the strength change degree, wherein the calculation modes of the strength change are as follows: strength change (tensile strength after soaking-tensile strength before soaking)/tensile strength before soaking. The larger the diameter change degree value is, the smaller the strength change degree value is, and the better the water response performance of the composite material is.
(5) Recovery performance
Cutting the rubber composite material into small pieces of 5mm, hot-press forming again, measuring the tensile strength of the formed composite material, and calculating the recovery effect, namely the tensile strength after the reshaping/the tensile strength before cutting, wherein the larger the numerical value is, the better the recovery effect is.
Example 1
The method comprises the following steps: preparing 300mL of 5wt% sodium hydroxide/15 wt% urea mixed solution, adding 30 parts by mass of 2000-mesh bacterial cellulose, and performing ultrasonic treatment at 500W for 1h to obtain a bacterial cellulose solution;
step two: adding 5 parts by mass of polyvinyl alcohol with the molecular weight of 10000 and the alcoholysis degree of 90% into 500mL of deionized water, heating to 95 ℃, stirring for 1h to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing ultrasonic treatment for 1h at 500W to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 25 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 1h to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, wherein the rubber latex is styrene butadiene rubber, the corresponding amount of dry rubber is 100 parts by mass, performing ultrasonic treatment for 2h at 500W, adding the aqueous dispersion obtained in the step two, continuing performing ultrasonic treatment for 0.5h, performing spray drying on the obtained mixed solution to obtain rubber powder, and performing hot pressing on the powder at 140 ℃ and 1.5MPa for 20min to obtain the multifunctional rubber composite material containing bacterial cellulose. The preparation flow chart is shown in figure 1. The three-dimensional network structure of the bacterial cellulose used is shown in fig. 2.
The rubber composite obtained was subjected to the following performance tests, and the performance results are shown in table 1.
Example 2
The method comprises the following steps: preparing 300mL of 5wt% sodium hydroxide/15 wt% urea mixed solution, adding 30 parts by mass of 2000-mesh bacterial cellulose, and performing ultrasonic treatment at 500W for 1h to obtain a bacterial cellulose solution;
step two: adding 5 parts by mass of polyvinyl alcohol with the molecular weight of 10000 and the alcoholysis degree of 90% into 500mL of deionized water, heating to 95 ℃, stirring for 2h to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing ultrasonic treatment at 500W for 1h to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 45 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 1h to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, wherein the rubber latex is natural rubber, the corresponding dry rubber dosage is 100 parts by mass, carrying out ultrasonic treatment at 750W for 1.5h, adding the aqueous dispersion obtained in the step two, continuing ultrasonic treatment for 0.5h, carrying out spray drying on the obtained mixed solution to obtain rubber powder, and carrying out hot pressing on the powder at 130 ℃ and 0.5MPa for 10min to obtain the multifunctional rubber composite material containing bacterial cellulose.
The rubber composite obtained was subjected to the following performance tests, and the performance results are shown in table 1.
Example 3
The method comprises the following steps: preparing 300mL of 10wt% sodium hydroxide/7 wt% urea mixed solution, adding 70 parts of 2000-mesh bacterial cellulose, and performing ultrasonic treatment at 1000W for 1h to obtain a bacterial cellulose solution;
step two: adding 20 parts by mass of polyvinyl alcohol with the molecular weight of 10000 and the alcoholysis degree of 98% into 500mL of deionized water, heating to 95 ℃, stirring for 3 hours to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing 1000W ultrasonic treatment for 0.5 hour to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 30 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 3h to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, wherein the rubber latex is nitrile rubber, the corresponding amount of dry rubber is 100 parts by mass, performing ultrasonic treatment for 1000W for 1h, adding the aqueous dispersion obtained in the step two, continuing performing ultrasonic treatment for 1h, performing spray drying on the obtained mixed solution to obtain rubber powder, and performing hot pressing on the powder at 140 ℃ and 1.5MPa for 20min to obtain the multifunctional rubber composite material containing bacterial cellulose.
The rubber composite obtained was subjected to the following performance tests, and the performance results are shown in table 1.
Example 4
The method comprises the following steps: preparing 300mL of 10wt% sodium hydroxide/7 wt% urea mixed solution, adding 30 parts of 2000-mesh bacterial cellulose, and performing ultrasonic treatment at 1000W for 1h to obtain a bacterial cellulose solution;
step two: adding 20 parts by mass of polyvinyl alcohol with the molecular weight of 10000 and the alcoholysis degree of 98% into 500mL of deionized water, heating to 95 ℃, stirring for 3 hours to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing 1000W ultrasonic treatment for 0.5 hour to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 30 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 3h to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, performing ultrasonic treatment for 1000W for 1h to obtain a rubber latex nitrile rubber, adding the aqueous dispersion obtained in the step two, continuing the ultrasonic treatment for 1h, performing spray drying on the obtained mixed solution to obtain rubber powder, and performing hot pressing on the powder at 140 ℃ and 1.5MPa for 20min to obtain the multifunctional rubber composite material containing bacterial cellulose.
The rubber composite obtained was subjected to the following performance tests, and the performance results are shown in table 1.
Example 5
The method comprises the following steps: preparing 300mL of 5wt% sodium hydroxide/15 wt% urea mixed solution, adding 70 parts of 2000-mesh bacterial cellulose, and performing ultrasonic treatment at 500W for 1h to obtain a bacterial cellulose solution;
step two: adding 5 parts by mass of polyvinyl alcohol with the molecular weight of 10000 and the alcoholysis degree of 90% into 500mL of deionized water, heating to 95 ℃, stirring for 1h to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing ultrasonic treatment for 1h at 500W to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 45 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 2h to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, wherein the rubber latex is natural rubber, the corresponding dry rubber dosage is 100 parts by mass, carrying out ultrasonic treatment at 750W for 1.5h, adding the aqueous dispersion obtained in the step two, continuing ultrasonic treatment for 0.5h, carrying out spray drying on the obtained mixed solution to obtain rubber powder, and carrying out hot pressing on the powder at 130 ℃ and 0.5MPa for 10min to obtain the multifunctional rubber composite material containing bacterial cellulose.
The rubber composite obtained was subjected to the following performance tests, and the performance results are shown in table 1.
Example 6
The method comprises the following steps: preparing 300mL of 5wt% sodium hydroxide/15 wt% urea mixed solution, adding 70 parts by mass of 2000-mesh bacterial cellulose, and performing ultrasonic treatment at 500W for 1h to obtain a bacterial cellulose solution;
step two: adding 5 parts by mass of polyvinyl alcohol with the molecular weight of 10000 and the alcoholysis degree of 90% into 500mL of deionized water, heating to 95 ℃, stirring for 1h to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and performing ultrasonic treatment for 1h at 500W to obtain a polyvinyl alcohol modified bacterial cellulose aqueous dispersion;
step three: adding 25 parts by mass of polyvinyl alcohol into 500mL of deionized water, heating to 95 ℃, stirring for 1h to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, wherein the rubber latex is styrene butadiene rubber, the corresponding amount of dry rubber is 100 parts by mass, performing ultrasonic treatment for 2h at 500W, adding the aqueous dispersion obtained in the step two, continuing performing ultrasonic treatment for 0.5h, performing spray drying on the obtained mixed solution to obtain rubber powder, and performing hot pressing on the powder at 140 ℃ and 1.5MPa for 20min to obtain the multifunctional rubber composite material containing bacterial cellulose.
The rubber composite obtained was subjected to the following performance tests, and the performance results are shown in table 1.
Comparative example 1
The method of example 1 was repeated at the specified contents of the respective components, but in step one, no bacterial cellulose was added, and the properties of the resulting rubber composite material were as shown in Table 1.
Comparative example 2
The method of example 2 was repeated at the specified contents of the respective components, but in step one, no bacterial cellulose was added, and the properties of the resulting rubber composite material were as shown in Table 1.
Comparative example 3
The method of example 3 was repeated at the specified contents of the respective components, but in step one, no bacterial cellulose was added, and the properties of the resulting rubber composite material were as shown in Table 1.
Comparative example 4
The method of example 3 was repeated at the specified contents of the respective components, but in the first and second steps, polyvinyl alcohol was not added, and the properties of the resulting rubber composite were as shown in Table 1.
Comparative example 5
The process of example 3 was repeated at the specified contents of the respective components, but in step one, polyvinyl alcohol was not added, and the properties of the resulting rubber composite were as shown in Table 1.
Comparative example 6
The method of example 3 was repeated at the specified contents of the respective components, but the bacterial cellulose, polyvinyl alcohol and latex were directly mixed in one step, and the properties of the resulting rubber composite material were as shown in Table 1.
TABLE 1
As can be seen from the above Table 1, the multifunctional rubber composite material containing bacterial cellulose has excellent properties such as high mechanical properties, good water responsiveness, good recycling effect and the like.
Claims (10)
1. The multifunctional rubber composite material containing the bacterial cellulose is characterized in that the multifunctional rubber containing the bacterial cellulose consists of 30-70 parts by mass of the bacterial cellulose, 100 parts by mass of rubber and 30-50 parts by mass of polyvinyl alcohol;
the multifunctional rubber containing bacterial cellulose is prepared by the following steps:
the method comprises the following steps: preparing a mixed solution of 5-10wt% of sodium hydroxide and 7-15wt% of urea, adding 30-70 parts of bacterial cellulose, and performing ultrasonic dispersion uniformly to obtain a bacterial cellulose solution;
step two: adding 5-20 parts by mass of polyvinyl alcohol into water, heating and stirring to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and uniformly dispersing by ultrasonic to obtain a polyvinyl alcohol modified bacterial cellulose water dispersion solution;
step three: adding 25-45 parts by mass of polyvinyl alcohol into water, heating and stirring to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, uniformly dispersing by ultrasonic, adding the polyvinyl alcohol modified bacterial cellulose aqueous dispersion obtained in the step two, continuously dispersing by ultrasonic, carrying out spray drying on the obtained mixed solution to obtain rubber powder, and carrying out hot pressing on the powder at the temperature of 130-140 ℃ and the pressure of 0.5-1.5MPa for 10-20min to obtain the multifunctional rubber composite material containing the bacterial cellulose.
2. The composite material of claim 1, wherein the bacterial cellulose has a size of 1000-2000 mesh.
3. The composite material of claim 1, wherein the rubber is any one of styrene butadiene rubber, natural rubber or nitrile butadiene rubber.
4. The composite material of claim 1, wherein the polyvinyl alcohol has a molecular weight of 5000-10000 and an alcoholysis degree of 90-98%.
5. A method for preparing a multifunctional rubber composite material containing bacterial cellulose as claimed in claim 1, comprising the steps of:
the method comprises the following steps: preparing a mixed solution of 5-10wt% of sodium hydroxide and 7-15wt% of urea, adding 30-70 parts of bacterial cellulose, and performing ultrasonic dispersion uniformly to obtain a bacterial cellulose solution;
step two: adding 5-20 parts by mass of polyvinyl alcohol into water, heating and stirring to obtain a polyvinyl alcohol solution, dropwise adding the bacterial cellulose solution obtained in the step one into the polyvinyl alcohol solution, and uniformly dispersing by ultrasonic to obtain a polyvinyl alcohol modified bacterial cellulose water dispersion solution;
step three: adding 25-45 parts by mass of polyvinyl alcohol into water, heating and stirring to obtain a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with rubber latex, uniformly dispersing by ultrasonic, adding the polyvinyl alcohol modified bacterial cellulose aqueous dispersion obtained in the step two, continuously dispersing by ultrasonic, carrying out spray drying on the obtained mixed solution to obtain rubber powder, and carrying out hot pressing on the powder at the temperature of 130-140 ℃ and the pressure of 0.5-1.5MPa for 10-20min to obtain the multifunctional rubber composite material containing the bacterial cellulose.
6. The method as claimed in claim 5, wherein in the step one, the ultrasound is performed at 500- > 1000W for 0.5-1 h.
7. The method of claim 5, wherein in step two, the mixture is heated to 95 ℃ and stirred for 1-3h to obtain the polyvinyl alcohol solution.
8. The method as claimed in claim 5, wherein in the second step, the ultrasound is performed at 500- > 1000W for 0.5-1 h.
9. The method of claim 5, wherein in step three, the mixture is heated to 95 ℃ and stirred for 1-3h to obtain the polyvinyl alcohol solution.
10. The method of claim 5, wherein in step three, the ultrasound is performed at 500- > 1000W for 1-2 h.
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