CN-118909335-B - Solid-phase regenerated rubber and preparation method and application thereof

CN118909335BCN 118909335 BCN118909335 BCN 118909335BCN-118909335-B

Abstract

The embodiment of the application relates to solid-phase regenerated rubber, and a preparation method and application thereof, and belongs to the technical field of waste rubber recycling. The solid-phase regenerated rubber comprises, by weight, 1-100 parts of waste rubber and 0.1-20 parts of diazonium compound/inverse vulcanized copolymer. According to the application, the specific compound or polymer with the C-H bond functionalization function is adopted as the interface modifier, so that the tensile strength of the solid-phase regenerated rubber and the tensile strength and fatigue threshold of the solid-phase regenerated rubber can be remarkably improved under the specific accelerator, a new means is provided for upgrading and recycling the waste rubber, and the method has a good application prospect.

Inventors

LUO MINGCHAO
Guo Haojia
ZHOU YU
HU BENXIANG
LIAO SHUANGQUAN

Assignees

海南大学

Dates

Publication Date: 20260512
Application Date: 20240724

Claims (4)

1. The solid-phase regenerated rubber is characterized by comprising the following preparation raw materials, by weight, 100 parts of primary rubber, 1-60 parts of waste rubber and 0.1-20 parts of diazonium compound; The primary rubber is natural rubber or synthetic rubber; the waste rubber is factory grade waste rubber; The diazonium compound is a diazonium compound containing a dynamic disulfide bond or a covalent bond; the preparation method of the solid-phase regenerated rubber comprises the following steps: s1, preparing a diazo compound containing dynamic disulfide bonds, namely dissolving 2-hydroxyethyl disulfide, pyridine and phenylacetyl chloride in dichloromethane, reacting at room temperature, purifying to obtain a first-step product, dissolving the first-step product, tosyl azide and 1, 8-diazabicyclo [5.4.0] undec-7-ene in dichloromethane, reacting at room temperature, purifying to obtain the diazo compound containing dynamic disulfide bonds, or Preparing a covalent bond-containing diazonium compound, namely dissolving ethylene glycol, pyridine and phenylacetyl chloride in dichloromethane, reacting at room temperature, purifying to obtain a first-step product, dissolving the first-step product, tosyl azide and 1, 8-diazabicyclo [5.4.0] undec-7-ene in dichloromethane, reacting at room temperature, and purifying to obtain the covalent bond-containing diazonium compound; S2, preparing solid-phase regenerated rubber, namely mixing the diazo compound containing dynamic disulfide bonds or covalent bonds, the primary rubber and the waste rubber, and performing hot press vulcanization at 100-145 ℃ for 15-30min under the vulcanization pressure of 10-15MPa to obtain the solid-phase regenerated rubber.
2. The solid phase reclaimed rubber of claim 1, wherein the virgin rubber is at least one of isoprene rubber, styrene butadiene rubber, nitrile butadiene rubber, butyl rubber, ethylene propylene rubber, and neoprene rubber.
3. The solid-phase reclaimed rubber as claimed in claim 1, wherein in the step S1, the ratio of the amounts of the substances of 2-hydroxyethyl disulfide, pyridine and phenylacetyl chloride is 1 (0.5-6), the ratio of the amounts of the substances of ethylene glycol, pyridine and phenylacetyl chloride is 1 (0.5-6), the ratio of the amounts of the substances of the first step product, tosyl azide and 1, 8-diazabicyclo [5.4.0] undec-7-ene is 1 (0.5-6), and the ratio of the amounts of the substances of ethylene glycol, pyridine and phenylacetyl chloride is 1 (0.5-6), respectively (0.5-6).
4. Use of a solid phase reclaimed rubber according to any one of claims 1-3 for the preparation of gaskets, rubber blends or equipment for tires or bridge engineering materials.

Description

Solid-phase regenerated rubber and preparation method and application thereof Technical Field The embodiment of the application relates to the technical field of waste rubber recycling, in particular to solid-phase regenerated rubber and a preparation method and application thereof. Background Because of its unique high elasticity, rubber is widely used in the fields of aerospace, national defense and military industry, tires, medical elastomers and the like, and plays a very important role in national economy construction. However, such widespread use also brings about tremendous recovery pressures. About 40 hundred million junked tires are discarded or left unused worldwide. The global recovery of waste rubber greatly affects the environment, energy and climate, and has resulted in "black pollution" which is more difficult to treat than "white pollution". At present, the recovery means of the waste rubber are mainly "degradation recovery", such as destruction by mechanical force, recovery and reuse as low value material. The production of reclaimed rubber is a main mode of high-valued recovery of waste rubber, however, the desulfurization and regeneration technology inevitably leads to the breakage of the main chain of a rubber molecular chain, so that the reclaimed rubber performance is reduced, and the defects of high pollution, high energy consumption and the like are accompanied. In addition, due to the characteristic that the sulfur vulcanization network can not be processed any more, the waste rubber used as the filler is blended with the primary rubber or other matrixes to cause phase separation phenomenon, so that the performance of the composite material is greatly reduced. Disclosure of Invention In view of the above, the embodiment of the application provides a solid-phase regenerated rubber, and a preparation method and application thereof, wherein the solid-phase regenerated rubber has better tensile strength and can effectively overcome the defects in the prior art. The embodiment of the application provides solid-phase regenerated rubber, which comprises 1-100 parts of waste rubber and 0.1-20 parts of diazonium compound/inverse vulcanized copolymer in parts by weight. In some embodiments, which can include the embodiments described above, the preparation materials include, by weight, 100 parts of virgin rubber, 0.1-20 parts of reverse vulcanized copolymer, 1-10 parts of zinc oxide, 1-5 parts of stearic acid, 1-5 parts of accelerator, 0.1-6 parts of sulfur, and 1-60 parts of waste rubber. In some embodiments, which may include the above embodiments, the raw materials for preparation include, by weight, 100 parts of virgin rubber, 0.1-20 parts of diazonium compound, and 1-60 parts of waste rubber. In some embodiments, which may include the above embodiments, the reverse-vulcanized copolymer is at least one of a hydroxyl-based reverse-vulcanized copolymer, a lipoic acid-based reverse-vulcanized copolymer, and a carboxyl-based reverse-vulcanized copolymer. In some embodiments, which may include the embodiments described above, the diazonium compound is a diazonium compound comprising a dynamic disulfide bond or a covalent bond. In some embodiments, which may include the above embodiments, the virgin rubber is natural rubber or synthetic rubber, or The primary rubber is at least one of isoprene rubber, styrene butadiene rubber, nitrile butadiene rubber, butyl rubber, ethylene propylene rubber and chloroprene rubber, or The waste rubber is factory grade waste rubber. The second aspect of the embodiment of the application also provides a preparation method of the solid-phase regenerated rubber, which comprises the following steps: S1, preparing a diazo compound, namely dissolving 2-hydroxyethyl disulfide (preferably bis (2-hydroxyethyl) disulfide)/ethylene glycol, pyridine and phenylacetyl chloride into dichloromethane, reacting for 1-12 hours at room temperature, purifying to obtain a first-step product, dissolving the first-step product, tosyl azide and 1, 8-diazabicyclo [5.4.0] undec-7-ene into dichloromethane, reacting for 1-12 hours at room temperature, and purifying to obtain the diazo compound; S2, preparing solid-phase regenerated rubber, namely mixing the diazo compound with waste rubber or mixing the diazo compound, the primary rubber and the waste rubber, and performing hot press vulcanization at 100-145 ℃ for 15-30min under the vulcanization pressure of 10-15MPa to obtain the solid-phase regenerated rubber. In some embodiments, which may include the above embodiments, the ratio of the amounts of the 2-hydroxyethyl disulfide/ethylene glycol, pyridine and phenylacetyl chloride is 1 (0.5-6): 0.5-6, and the ratio of the amounts of the first step product, tosyl azide and 1, 8-diazabicyclo [5.4.0] undec-7-ene is 1 (0.5-6): 0.5-6, in step S1. The third aspect of the embodiment of the application also provides a preparation method of the solid-phase regenerated rubber, which comprises the foll