CN115926464B - Preparation method of silicon rubber reinforced particles and reinforced rubber powder - Google Patents
Preparation method of silicon rubber reinforced particles and reinforced rubber powder Download PDFInfo
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Abstract
The invention belongs to the technical field of composite materials and rubber powder preparation, and discloses a preparation method of silicon rubber reinforced particles and reinforced rubber powder. The preparation method of the silicon rubber reinforced particles and the reinforced rubber powder comprises the following steps: and (3) carrying out hydrosilylation reaction on hydrogen-containing silicone oil and aliphatic hydrocarbon containing at least two unsaturated groups to obtain a cross-linked polysiloxane elastomer solution, adding silica sol, stirring and mixing uniformly, vacuum drying, crushing and sieving to obtain the silicone rubber reinforced particles. Cleaning waste tires, cutting into pieces, crushing, sieving, magnetically separating to obtain rubber powder, and mixing with silicon rubber reinforced particles to obtain reinforced rubber powder. The invention uses specific silicon rubber reinforced particles to reinforce the regenerated rubber powder, can obviously improve the mechanical property of the rubber powder, widens the application field of the regenerated rubber powder, can realize the recycling of waste rubber materials such as waste tires and the like, and obviously increases the economic benefit and the environmental protection benefit.
Description
Technical Field
The invention belongs to the technical field of preparation of composite materials and rubber powder, and particularly relates to a preparation method of silicon rubber reinforced particles and reinforced rubber powder.
Background
Rubber powder is generally processed from junked tires or junked rubber products. The processing method adopted in common comprises the following steps: normal temperature pulverizing method, freezing method, normal temperature chemical method, etc. The rubber powder is a main raw material of reclaimed rubber, is widely used in the fields of sports plastic stadium, recreation ground, rubber floor tile, waterproof coiled material, waterproof coating, highway modified asphalt, rubber products and the like, and can also be directly used as rubber products.
However, due to the common problems of ageing, degradation and the like of the waste tires or the waste rubber products, the mechanical properties of the rubber powder prepared from the waste tires or the waste rubber products are obviously reduced compared with those of primary rubber, so that the application field is limited. Therefore, studies on improving the use properties of rubber powders by modifying the rubber powders through physical or chemical methods are increasing.
In our earlier patent CN 109774016A a method for producing fine rubber powder from junked tires is disclosed. The conventional normal-temperature rubber powder production process is optimized, and a multi-stage screening module is added in the coarse crushing and fine crushing processes, so that the efficient utilization of raw materials is ensured, and the utilization rate of the raw materials and the generation rate of fine rubber powder are improved; calcium carbonate powder and circuit board powder are added in the preparation of the abrasive, so that the fluidity and dispersibility of the rubber powder in the crushing process are effectively promoted, the rubber powder is not easy to agglomerate, and the geometrical physical properties of the rubber powder are not influenced.
Patent CN 111662031A discloses a method for modifying rubber powder by using polyphenols, which comprises the following steps: step one, preparing polyphenol substance dispersion liquid; and step two, adding rubber powder into the polyphenol substance dispersion liquid, heating and stirring, filtering the materials after the reaction is finished, and drying the filtered solid in a drying oven to obtain the modified rubber powder. The invention mainly aims to improve the hydrophilic performance of rubber powder by forming a coating on the surface of the rubber powder through chemical reaction of the polyphenol substances, but the modification method does not obviously improve the mechanical properties such as strength and the like of the rubber powder.
Patent CN 115159902A discloses a preparation method of modified rubber powder, wherein waste rubber powder is treated by alkaline aqueous solution and then oxidized by potassium permanganate aqueous solution under acidic condition; then, carrying out sulfonation treatment by using dodecyl benzene sulfonic acid solution; and (5) coating the rubber powder by peach resin, and finally crushing. The invention adopts potassium permanganate aqueous solution to oxidize rubber powder under acidic condition, then adopts dodecylbenzene sulfonic acid solution to sulfonate, and introduces oxygen-containing groups and sulfonic groups respectively, thereby improving the hydrophilicity of the rubber powder; finally, the peach resin is used for coating the rubber powder to form a composite structure with the organic waste rubber powder as a core and the organic peach resin as a shell. The mechanical properties of the rubber powder are improved through multistage treatment.
The silicone rubber has good mechanical property and weather resistance, and chemical or physical blending modification of the rubber powder by the silicone rubber is a good prospect, but the silicone rubber has high chemical modification difficulty and poor physical blending modification effect due to poor compatibility of polysiloxane chains and organic rubber materials.
Disclosure of Invention
In view of the above drawbacks and shortcomings of the prior art, a primary object of the present invention is to provide a method for preparing silicone rubber reinforced particles.
Another object of the present invention is to provide a silicone rubber reinforcing particle prepared by the above method.
Still another object of the present invention is to provide a method for preparing the reinforced rubber powder.
The invention aims at realizing the following technical scheme:
a preparation method of silicone rubber reinforced particles comprises the following preparation steps:
(1) Adding hydrogen-containing silicone oil and aliphatic hydrocarbon containing at least two unsaturated groups into an organic solvent, stirring and dissolving uniformly, heating to 75-95 ℃ under the protection of inert atmosphere, and then adding a catalyst, stirring and reacting until the hydrosilylation reaction is complete;
(2) Adding silica sol into the reaction liquid in the step (1), stirring and mixing uniformly, vacuum drying to remove the organic solvent, grinding and crushing the product, and sieving to obtain SiO 2 -cross-linked silicone composite structured silicone rubber reinforcing particles.
Further, the hydrogen content (mass percent) of the hydrogen-containing silicone oil in the step (1) is 0.05-2%.
Further, the aliphatic hydrocarbon containing at least two unsaturated groups in the step (1) is selected from one or a combination of at least two of 1, 3-butadiene, 1, 4-pentadiene, 1, 5-hexadiene, 1, 6-heptadiene, 1, 7-octadiene, 1, 8-nonadiene, 1, 9-decadiene, 1, 10-undecadiene and 1, 11-dodecadiene; the addition amount of the aliphatic hydrocarbon containing at least two unsaturated groups is 5-30% of the mass of the hydrogen-containing silicone oil.
Further, the organic solvent in the step (1) is at least one of isopropanol, isobutanol and isoparaffin, and more preferably a mixed solvent of isopropanol and isoparaffin.
Further, the catalyst in the step (1) is a vinyl platinum complex or chloroplatinic acid.
Further, the reaction time in the step (1) is 1 to 6 hours.
Further, the silica sol in step (2) is preferably a solvent-type hydrophobic silica sol; the addition amount of the silica sol is 60-200% of the mass of the hydrogen-containing silicone oil based on the solid content. The test of the invention finds that the addition of the silica sol is too low, which can cause the adhesion of the crosslinked polysiloxane, is unfavorable for grinding and crushing to obtain well-dispersed powder, and is not easy to mix with rubber powder for reinforcement; too high an amount may result in a decrease in the reinforcing effect of the resulting reinforcing particles on the rubber powder.
Further, the sieving in the step (2) means passing through a 60-200 mesh screen.
The silicon rubber reinforced particles are prepared by the method.
The preparation method of the reinforced rubber powder comprises the following preparation steps:
1) Cleaning, dicing, crushing, sieving and magnetically separating the waste tires to obtain rubber powder;
2) And (2) adding the silicon rubber reinforced particles into the rubber powder in the step (1) according to a certain proportion to obtain the reinforced rubber powder.
Further, in the step 1), the sieving refers to passing through a 60-200 mesh screen; the addition amount of the silicon rubber reinforced particles in the step 2) is 2-20% of the mass of the rubber powder.
The principle of the invention is as follows: the cross-linked elastomer containing long-chain polysiloxane is prepared by performing hydrosilylation reaction on aliphatic hydrocarbon containing at least two unsaturated groups and hydrogen-containing silicone oil, and the cross-linked polysiloxane elastomer structure can obviously improve the mechanical properties of the organic rubber powder. Meanwhile, the aliphatic hydrocarbon containing at least two unsaturated groups has good compatibility with the organic rubber powder, so that the defect that polysiloxane is incompatible with the organic rubber powder is overcome to a certain extent, and the advantage performance of the crosslinked polysiloxane elastomer is well exerted in the organic rubber powder. The silica sol is added to form SiO with the cross-linked polysiloxane elastomer 2 -intersection ofThe bipolysiloxane composite structure has the advantages that one of the functions is to reduce the adhesion of the crosslinked polysiloxane elastomer, so that the powder with good dispersion is easily obtained, and the mixture and the addition of the bipolysiloxane composite structure and the organic rubber powder are convenient; the second effect is to further improve the modification effect of the cross-linked polysiloxane elastomer on the organic rubber powder, and the test proves that the composite of the cross-linked polysiloxane elastomer and the organic rubber powder has obvious synergistic effect on improving the mechanical property of the organic rubber powder.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses specific silicon rubber reinforced particles to reinforce the regenerated rubber powder, can obviously improve the mechanical property of the rubber powder, widens the application field of the regenerated rubber powder, can realize the recycling of waste rubber materials such as waste tires and the like, and obviously increases the economic benefit and the environmental protection benefit.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
The preparation method of the reinforced rubber powder comprises the following preparation steps:
1) Cleaning waste tires, cutting the waste tires into pieces, crushing the waste tires, sieving the waste tires with a 80-mesh sieve, and magnetically separating the waste tires to remove metal impurities in rubber particles to obtain rubber powder;
2) And (3) adding the silicon rubber reinforced particles into the rubber powder in the step (1) in a mass percentage of 6%, so as to obtain the reinforced rubber powder.
The silicone rubber reinforced particles of the embodiment are prepared by the following method:
(1) 500g of hydrogen-containing silicone oil (hydrogen content is 0.53%) and 100g of 1, 6-heptadiene are added into 1.5kg of mixed solvent of isopropanol and isoparaffin, stirred and dissolved uniformly, the temperature is raised to 85 ℃ under the protection of nitrogen, and then a catalytic amount of vinyl platinum complex solution is added for stirring and reacting for 4 hours, so that the cross-linked polysiloxane elastomer solution is obtained.
(2) Adding solvent-type hydrophobic silica sol (30% of silicon dioxide content, 15-25 nm of particle diameter and 1.2 mPa.s of viscosity) into the reaction solution in the step (1) and stirringMixing, vacuum drying to remove organic solvent, grinding, pulverizing, sieving with 80 mesh sieve to obtain SiO 2 -cross-linked silicone composite structured silicone rubber reinforcing particles.
The addition amount of the solvent type hydrophobic silica sol is respectively adjusted to be 0%, 30%, 60%, 90%, 150%, 200% and 250% of the mass of the hydrogen-containing silicone oil based on the content of silicon dioxide. The processing performance (passing rate of 80 mesh screen after grinding and crushing under the same condition) of the obtained silicon rubber reinforced particles is compared with the mechanical performance of the obtained reinforced rubber powder, the obtained rubber powder of each group is subjected to sheeting and film pressing according to a test formula of tensile strength and elongation at break in GB/T19208-2020, the tensile strength and elongation at break are tested according to GB/T528-2009 after film pressing, and in addition, the aclonal abrasion performance of the product after film pressing is tested according to GBT 1689-2014. The test results are shown in table 1 below, with the rubber powder without added silicone rubber reinforcing particles as a control.
TABLE 1
| Test item | Pass rate of | Tensile Strength | Elongation at break | Acle abrasion |
| 0％ | 6.2％ | 36.2MPa | 654％ | 0.2235 |
| 30％ | 57.5％ | 41.7MPa | 682％ | 0.1832 |
| 60％ | 90.8％ | 47.4MPa | 665％ | 0.1526 |
| 90％ | 95.8％ | 47.5MPa | 630％ | 0.1370 |
| 150％ | 97.3％ | 46.2MPa | 606％ | 0.1253 |
| 200％ | 97.9％ | 42.8MPa | 575％ | 0.1189 |
| 250％ | 98.2％ | 36.9MPa | 562％ | 0.1107 |
| Control group | ---- | 28.8MPa | 480％ | 0.3652 |
As can be seen from the results in Table 1, compared with the control group, the simple cross-linked polysiloxane elastomer obtained without adding silica sol (0%) has an obvious improvement effect on the mechanical properties of the rubber powder, but the addition of no silica sol or too low of silica sol can cause the cross-linked polysiloxane to adhere, which is not beneficial to grinding and crushing to obtain well-dispersed powder, and the processability of the obtained silicone rubber reinforced particles is poor. Compared with the group without adding the silica sol (0%) and the group with excessively high addition amount of the silica sol (250%), the improvement effect (especially the tensile strength and the elongation at break) of the rubber powder mechanical property of the composite of the silica sol and the silica sol is further obviously improved, which proves that the composite of the silica sol and the rubber powder has obvious synergistic effect on the improvement of the organic rubber powder mechanical property.
Comparative example 1
In this comparative example, compared with example 1, nano SiO was used in the preparation of the silicone rubber reinforced particles 2 The powder replaces silica sol, and the rest are the same.
The silicon rubber reinforced particles are prepared by the following method:
(1) 500g of hydrogen-containing silicone oil (hydrogen content is 0.53%) and 100g of 1, 6-heptadiene are added into 1.5kg of mixed solvent of isopropanol and isoparaffin, stirred and dissolved uniformly, the temperature is raised to 85 ℃ under the protection of nitrogen, and then a catalytic amount of vinyl platinum complex solution is added for stirring and reacting for 4 hours, so that the cross-linked polysiloxane elastomer solution is obtained.
(2) Adding nano SiO into the reaction liquid in the step (1) 2 Powder is stirred and mixed uniformly, and nano SiO 2 The adding amount of the powder is 90% of the mass of the hydrogen-containing silicone oil, the organic solvent is removed by vacuum drying, the product is ground and crushed, and the product is filtered by a 80-mesh screen to obtain the SiO coated by the cross-linked polysiloxane elastomer 2 Is a silicone rubber reinforcing particle.
The processability of the silicone rubber reinforced particles obtained in this comparative example showed a sieving pass rate of 45.3%, indicating that the crosslinked polysiloxane elastomer coated SiO 2 The structure of (3) still has obvious cross-linked polysiloxane adhesion.
The mechanical property test of the reinforced rubber powder obtained in the comparative example shows that the tensile strength is 37.4MPa, the elongation at break is 557% and the Aldrich abrasion is 0.2053. The comparison with example 1 further demonstrates that the composite structure formed by the cross-linked polysiloxane elastomer and the silica sol has a significant synergistic effect on the improvement of the mechanical properties of the rubber powder.
Comparative example 2
This comparative example uses a hydrophilic silica sol instead of a solvent-type hydrophobic silica sol as compared to example 1, the remainder being the same.
The silicon rubber reinforced particles are prepared by the following method:
(1) 500g of hydrogen-containing silicone oil (hydrogen content is 0.53%) and 100g of 1, 6-heptadiene are added into 1.5kg of mixed solvent of isopropanol and isoparaffin, stirred and dissolved uniformly, the temperature is raised to 85 ℃ under the protection of nitrogen, and then a catalytic amount of vinyl platinum complex solution is added for stirring and reacting for 4 hours, so that the cross-linked polysiloxane elastomer solution is obtained.
(2) Adding hydrophilic silica sol (silica content: 25%; water content: 75%) into the reaction solution of the step (1), stirring and mixing uniformly, wherein the addition amount of the hydrophilic silica sol is 90% of the mass of the hydrogen-containing silicone oil based on the silica content, vacuum drying to remove water and organic solvent, grinding and crushing the product, and sieving with a 80-mesh sieve to obtain SiO 2 -cross-linked silicone composite structured silicone rubber reinforcing particles.
The processability of the silicone rubber reinforced particles obtained in this comparative example showed a sieving pass rate of 72.6%, indicating that some cross-linked polysiloxane adhesion still exists by compounding the hydrophilic silica sol with the cross-linked polysiloxane elastomer.
The mechanical property test of the reinforced rubber powder obtained in the comparative example shows that the tensile strength is 39.1MPa, the elongation at break is 572% and the Aldrich abrasion is 0.1856. The comparison with example 1 further demonstrates that the composite structure formed by the cross-linked polysiloxane elastomer and the hydrophobic silica sol has more obvious effect of improving the mechanical properties of the rubber powder. The reason for this may be that the hydrophilic silica sol has poor compatibility with the solution system of the crosslinked polysiloxane elastomer, and is prematurely agglomerated after addition, and a good composite structure with the crosslinked polysiloxane elastomer cannot be effectively formed, resulting in deterioration of processability of the silicone rubber reinforcing particles and deterioration of reinforcing performance on the rubber powder.
Example 2
The preparation method of the reinforced rubber powder comprises the following preparation steps:
1) Cleaning waste tires, cutting the waste tires into pieces, crushing the waste tires, sieving the waste tires with a 80-mesh sieve, and magnetically separating the waste tires to remove metal impurities in rubber particles to obtain rubber powder;
2) And (3) adding the silicon rubber reinforced particles into the rubber powder in the step (1) in a mass percentage of 2%, so as to obtain the reinforced rubber powder.
The silicone rubber reinforced particles of the embodiment are prepared by the following method:
(1) 500g of hydrogen-containing silicone oil (hydrogen content is 1.26%) and 150g of 1, 9-decadiene are added into a mixed solvent of 1.8kg of isopropanol and isoparaffin, stirred and dissolved uniformly, the temperature is raised to 80 ℃ under the protection of nitrogen, and then a catalytic amount of vinyl platinum complex solution is added for stirring and reacting for 3 hours, so that a cross-linked polysiloxane elastomer solution is obtained.
(2) Adding solvent-based hydrophobic silica sol (30% of silicon dioxide content, 15-25 nm of particle size and 1.2 mPa.s of viscosity) into the reaction solution in the step (1), stirring and mixing uniformly, wherein the addition amount of the hydrophobic silica sol is 100% of the mass of hydrogen-containing silicone oil based on the silicon dioxide content, removing the organic solvent by vacuum drying, grinding and crushing the product, and sieving the product with a 80-mesh sieve to obtain SiO 2 -cross-linked silicone composite structured silicone rubber reinforcing particles.
The processability of the silicone rubber reinforced particles obtained in this example showed a sieving passage of 96.8%; the mechanical property test result of the obtained reinforced rubber powder shows that the tensile strength is 43.3MPa, the elongation at break is 612%, and the acle abrasion is 0.1285.
Example 3
The preparation method of the reinforced rubber powder comprises the following preparation steps:
1) Cleaning waste tires, cutting the waste tires into pieces, crushing the waste tires, sieving the waste tires with a 80-mesh sieve, and magnetically separating the waste tires to remove metal impurities in rubber particles to obtain rubber powder;
2) And (3) adding the silicon rubber reinforced particles into the rubber powder in the step (1) in a mass percentage of 20%, so as to obtain the reinforced rubber powder.
The silicone rubber reinforced particles of the embodiment are prepared by the following method:
(1) 500g of hydrogen-containing silicone oil (hydrogen content is 0.083%) and 30g of 1, 4-pentadiene are added into a mixed solvent of 1.2kg of isopropanol and isoparaffin, stirred and dissolved uniformly, the temperature is raised to 90 ℃ under the protection of nitrogen, and then a catalytic amount of vinyl platinum complex solution is added for stirring and reacting for 5 hours, so that the cross-linked polysiloxane elastomer solution is obtained.
(2) Adding solvent-based hydrophobic silica sol (30% of silicon dioxide content, 15-25 nm of particle size and 1.2 mPa.s of viscosity) into the reaction solution in the step (1), stirring and mixing uniformly, wherein the addition amount of the hydrophobic silica sol is 120% of the mass of hydrogen-containing silicone oil based on the silicon dioxide content, removing the organic solvent by vacuum drying, grinding and crushing the product, and sieving the product with a 80-mesh sieve to obtain SiO 2 -cross-linked silicone composite structured silicone rubber reinforcing particles.
The processability of the silicone rubber reinforced particles obtained in this example showed a sieving passage of 95.2%; the mechanical property test result of the obtained reinforced rubber powder shows that the tensile strength is 46.8MPa, the elongation at break is 656%, and the Aldrich abrasion is 0.1310.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the silicon rubber reinforced particles is characterized by comprising the following preparation steps:
(1) Adding hydrogen-containing silicone oil and aliphatic hydrocarbon containing at least two unsaturated groups into an organic solvent, stirring and dissolving uniformly, heating to 75-95 ℃ under the protection of inert atmosphere, and then adding a catalyst, stirring and reacting until the hydrosilylation reaction is complete;
(2) Adding silica sol into the reaction liquid in the step (1), stirring and mixing uniformly, vacuum drying to remove the organic solvent, grinding and crushing the product, and sieving to obtain SiO 2 -silicone rubber reinforcing particles of crosslinked polysiloxane composite structure;
the aliphatic hydrocarbon containing at least two unsaturated groups in the step (1) is selected from one or a combination of at least two of 1, 3-butadiene, 1, 4-pentadiene, 1, 5-hexadiene, 1, 6-heptadiene, 1, 7-octadiene, 1, 8-nonadiene, 1, 9-decadiene, 1, 10-undecadiene and 1, 11-dodecadiene; the addition amount of the aliphatic hydrocarbon containing at least two unsaturated groups is 5% -30% of the mass of the hydrogen-containing silicone oil;
the silica sol in the step (2) is solvent type hydrophobic silica sol; the addition amount of the silica sol is 60% -200% of the mass of the hydrogen-containing silicone oil in terms of solid content.
2. The method for preparing silicone rubber reinforced particles according to claim 1, wherein the hydrogen content of the hydrogen-containing silicone oil in the step (1) is 0.05% -2%.
3. The method for producing a silicone rubber reinforcing particle according to claim 1, wherein the organic solvent in step (1) is at least one of isopropyl alcohol, isobutyl alcohol and isoparaffin; the catalyst is vinyl platinum complex or chloroplatinic acid; the stirring reaction time is 1-6 h.
4. A method for producing silicone rubber reinforced particles according to claim 3, wherein the organic solvent in step (1) is a mixed solvent of isopropyl alcohol and isoparaffin.
5. The method for preparing silicone rubber reinforced particles according to claim 1, wherein the sieving in the step (2) is performed by a 60-200 mesh sieve.
6. A silicone rubber reinforced particle prepared by the method of any one of claims 1 to 5.
7. The preparation method of the reinforced rubber powder is characterized by comprising the following preparation steps:
1) Cleaning, dicing, crushing, sieving and magnetically separating the waste tires to obtain rubber powder;
2) The silicone rubber reinforcing particles according to claim 6 are added to the rubber powder of step 1) in a certain proportion to obtain a reinforced rubber powder.
8. The method for preparing reinforced rubber powder according to claim 7, wherein the sieving in the step 1) is through a 60-200 mesh screen; the addition amount of the silicon rubber reinforced particles in the step 2) is 2% -20% of the mass of the rubber powder.
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