CN111205507A - Production method of high-performance environment-friendly reclaimed rubber - Google Patents
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- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
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- C08J11/26—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing carboxylic acid groups, their anhydrides or esters
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Abstract
The invention discloses a production method of high-performance environment-friendly reclaimed rubber, which comprises the following steps: (1) mixing palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 0.8-1.2: 2.5-4: 0.1-0.3, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:1-9 to form stable solution A; (2) carrying out wet cutting and grinding on waste rubber particles by adopting the solution A, and removing liquid to obtain activated rubber powder B; (3) and carrying out flash evaporation regeneration on the activated rubber powder B to obtain desulfurized rubber powder C, and plasticating to obtain regenerated rubber D. The invention carries out activation treatment on rubber powder while carrying out wet grinding, and solves the problems of performance loss and environmental pollution in the regeneration process of rubber through flash evaporation and desulfurization.
Description
Technical Field
The invention belongs to the technical field of reclaimed rubber, and particularly relates to a production method of high-performance environment-friendly reclaimed rubber.
Background
China is a country with scarce rubber resources, the renewable resources of rubber are indispensable sources for replacing imports in China, and the recycling of rubber is an imminent problem of solving the pollution of waste rubber in the world in large environment. The waste rubber in the world pollutes the land, the sea and the air more and more seriously, generates fire, pollutes water sources and other problems, China is a big country and a strong country producing reclaimed rubber in the world, the yield accounts for 90 percent of the world yield, and along with the world opening, the reclaimed rubber technology in China gradually branches and leaves in the world, but the technology producing reclaimed rubber in China still has some defects: 1. the pollution to products and environment is still serious in the production process; 2. the efficiency of the reduced vulcanized rubber of the reclaimed rubber is still not high; 3. the production mode still belongs to high energy consumption and low output. These problems have long limited and plagued the development of reclaimed rubber industry in our country.
The main body of the regeneration plasticizing technology is a thermal cracking method, namely rubber powder is obtained by a normal-temperature mechanical crushing method, then the rubber powder is placed in a desulfurizing tank, a dynamic desulfurizing tank and a screw rod for rotary extrusion or high-temperature pyrolysis, and an auxiliary agent is added for plasticizing and regenerating to obtain the regenerated rubber; in the plasticizing process, an auxiliary agent is not added, and the reclaimed rubber is obtained by an over-cracking method, so that the performance index of the reclaimed rubber obtained by the method is poorer, and only pollution is directly or indirectly transferred.
Chinese patent with publication number CN106867064B discloses an environment-friendly reclaimed rubber, which is prepared from waste rubber powder and auxiliary materials according to the weight ratio of 8-12: 1.5-3 by weight; the auxiliary materials are prepared from the following raw materials in parts by weight: 20-40 parts of palm oil, 4-6 parts of tall oil, 5-10 parts of a softening agent, 1-4 parts of an activating agent, 2-4 parts of ethylene glycol monoethyl ether acetate, 3-10 parts of oxidized polyethylene wax, 1-4 parts of stearic acid, 1-3 parts of sodium tripolyphosphate and 3-5 parts of papermaking sludge ash. The environment-friendly reclaimed rubber prepared by the method has the advantages of good tensile strength and elongation at break, small smell, no peculiar smell, no harmful substances and the like, can meet the standard requirements of miscellaneous rubber reclaimed rubber on the physical properties of density, ash content and the like of reclaimed rubber, is harmless to human bodies, can obviously improve various properties of reclaimed rubber, can be used for producing civil products, is safe and environment-friendly, and has wide market prospect. The Chinese patent application with publication number CN108102181A discloses a method for preparing reclaimed rubber from waste rubber particles, which comprises cleaning waste tires, drying, pulverizing, and sieving to obtain black rubber powder. Cleaning the leftover materials of the shoe soles, drying, crushing and sieving to obtain the yellow glue powder for later use. 50 parts of carbon black, 50 parts of black rubber powder and 50 parts of yellow rubber powder, performing high-temperature plastication on the rubber powder and the carbon black on a plasticator to prepare regenerated master batch, and then mixing the master batch with zinc oxide, stearic acid, a regenerant and an accelerant. Mixing, standing for 10-20h to obtain mixed rubber; and (3) putting the rubber compound into an open mill for vulcanization, adding an accelerator and sulfur, and performing thin-pass triangular bag making for 4-7 times to obtain a finished product. The invention adopts a high-temperature regeneration vulcanization method to prepare the reclaimed rubber, and has the advantages of environment-friendly preparation and simple operation. The preparation method of the invention increases the utilization rate of the waste rubber, reduces the rubber industrial garbage, ensures that the reclaimed rubber can reach the national or industrial standard, and has the advantages of waste utilization, environmental protection and the like. However, the desulfurization effect of the waste rubber in these patents is general, the whole preparation process is completed in different reactors, the precursor needs to be transferred to the next reaction vessel again in the middle, and the material loss is easy to generate in the process, and the environment is easy to be polluted.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a production method of high-performance environment-friendly reclaimed rubber.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) mixing palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 0.8-1.2: 2.5-4: 0.1-0.3, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:1-9 to form stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting the solution A, and removing liquid to obtain activated rubber powder B;
(3) and carrying out flash evaporation regeneration on the activated rubber powder B to obtain desulfurized rubber powder C, and plasticating to obtain regenerated rubber D.
Preferably, the waste rubber particles in the step (2) are tire tread vulcanized rubber whole tire particles, and the particle size is 5-10 meshes.
Preferably, the weight ratio of the waste rubber particles and the solution A in the step (2) is 1: 5-10.
Preferably, the particle size of the activated rubber powder B in the step (2) is 30-60 meshes.
Preferably, the liquid content of the activated rubber powder B in the step (2) is 10-15%.
Preferably, the flash evaporation conditions in step (3) are: the air inlet temperature is 380 ℃ minus 420 ℃, the air outlet temperature is 190 ℃ minus 210 ℃, and the time for passing through the flash channel is 1-1.5 min.
Preferably, the plastication temperature in the step (3) is less than or equal to 60 ℃.
The invention has the following positive beneficial effects:
the general regeneration plasticizing technology of the existing reclaimed rubber method has the main defects that: normal temperature mechanical pulverization is open operation, and dust pollution is difficult to effectively control on the one hand, and on the other hand lacks effectual cooling method, and rubber carries out the hot oxygen shearing and rolls under mechanical action, and rubber all can appear the carbonization because of hot oxygen ageing at this in-process to the performance of rubber constantly loses when constantly repeated rolling number of times. And the rubber powder has poor thermal conductivity and large friction force between rubber powders, so that the rubber powder has poor mixing performance with additives in the plasticizing and regenerating process, the uniformity of thermal cracking control is poor, the obtained regenerated rubber product has low stability, and the quality of the regenerated rubber product is poor. The invention solves the problem which can not be avoided in the conventional reclaimed rubber method, the produced reclaimed rubber has high performance and stable quality, the problems of performance loss and environmental pollution in the conventional rubber regeneration process are thoroughly solved, and the further explanation is as follows:
1. the invention adopts wet active modification (shallow desulfurization), obtains activation in the process of rubber powder grinding through wet grinding activation, simultaneously avoids performance loss and partial surface carbonization of vulcanized rubber in the conventional grinding process, ensures that the rubber powder keeps better performance before deep desulfurization, creatively moves the desulfurization stroke of the reclaimed rubber, ensures that the desulfurization process is not limited to desulfurization in the traditional sense, further adopts a flash evaporation method for desulfurization (deep desulfurization), ensures that the rubber powder takes hot air as a desulfurization heat transfer medium to ensure that the rubber powder is heated and transfers heat more evenly, thereby realizing more uniform desulfurization and more full desulfurization.
2. The invention adopts wet-method grinding rubber, the regeneration auxiliary agents of palm oil, naphthenic oil, rosin and petroleum sodium sulfonate and water are prepared into a stable water-soluble emulsion state to be used as a medium of rubber desulfurization auxiliary agent and wet-method grinding, the palm oil, the naphthenic oil, the rosin and the petroleum sodium sulfonate are matched to form a swelling and permeating system, the rubber powder is activated while the wet-method grinding is carried out, the desulfurization auxiliary agent is uniformly wrapped when the rubber powder is ground, the rubber powder is uniformly heated and uniformly permeated during flash evaporation to be plasticized and regenerated, the auxiliary agent and the rubber powder are fully mixed, and the wet-method grinding does not have the friction high-temperature phenomenon, thereby effectively controlling the thermal cracking process, avoiding the serious pollution problem caused by ineffective excessive softener and ultrahigh-temperature plasticizing over-cracking in the traditional plasticizing regeneration process, and avoiding the serious pollution problem caused by multiple times of thermal oxidation aging and overheating cracking of the rubber powder in, Elongation, elasticity, wear resistance and anti-bending property loss to obtain the environment-friendly reclaimed rubber with high reduction property, wherein the Mooney viscosity ML (1 + 4) of the reclaimed rubber is 55-65 N.m at 100 ℃, the tensile strength is 11.5-14.2MPa, the elongation at break is 355-385 percent, and the performance is excellent.
3. The invention takes hot air as a medium, and uses activated rubber powder for flash evaporation regeneration, so as to solve the problems of rubber powder that heat transfer, uniform heating and overheating and aging need to be protected at one time. The whole system can realize automatic sealing operation and effectively control pollution.
Detailed Description
The invention will be further illustrated with reference to some specific embodiments.
Example 1
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 0.8: 3: 0.1 mixing and emulsifying, and further mixing with water according to the weight ratio of 1:1 to form a stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the weight ratio of the waste rubber particles to the solution A is 1: 5, collecting rubber powder of 40 meshes, and centrifugally removing liquid to obtain activated rubber powder B with 15% of liquid content;
the waste rubber particles are tire tread vulcanized rubber full tire particles, and the particle size is 5 meshes;
(3) and (3) performing flash evaporation desulfurization on the activated rubber powder B, controlling the temperature of an air inlet medium to be 400 ℃ and the outlet temperature to be 190 ℃, passing through a flash evaporation passage for 1min to obtain desulfurized rubber powder C, performing conventional plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging to obtain regenerated rubber D.
Example 2
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, paraffin oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 1: 3.5: 0.2, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:1.5 to form a stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the weight ratio of the waste rubber particles to the solution A is 1: 6, collecting 50-mesh rubber powder, and centrifugally removing liquid to obtain activated rubber powder B with the liquid content of 12%;
the waste rubber particles are tire tread vulcanized rubber full tire particles, and the particle size is 5 meshes;
(3) and (3) performing flash evaporation desulfurization on the activated rubber powder B, controlling the temperature of an air inlet medium to be 400 ℃ and the outlet temperature to be 200 ℃, passing through a flash evaporation passage for 1min to obtain desulfurized rubber powder C, performing conventional plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging to obtain regenerated rubber D.
Example 3
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting tall oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 1: 3: 0.2 mixing and emulsifying, and further mixing with water according to the weight ratio of 1:2 to form stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the weight ratio of the waste rubber particles to the solution A is 1: 8, collecting 60-mesh rubber powder, and centrifugally removing liquid to obtain activated rubber powder B with the liquid content of 10%;
the waste rubber particles are tire tread vulcanized rubber full tire particles, and the particle size is 10 meshes;
(3) and (3) carrying out flash evaporation desulfurization on the activated rubber powder B, controlling the temperature of an air inlet medium to be 380 ℃ and the outlet temperature to be 200 ℃, passing through a flash evaporation passage for 1.2min to obtain desulfurized rubber powder C, carrying out conventional plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging to obtain regenerated rubber D.
Example 4
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 1: 3: 0.2, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:4 to form a stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the weight ratio of the waste rubber particles to the solution A is 1: 8, collecting rubber powder of 40 meshes, and centrifugally removing liquid to obtain activated rubber powder B with 15% of liquid content;
the waste rubber particles are tire tread vulcanized rubber full tire particles, and the particle size is 5 meshes;
(3) and (3) performing flash evaporation desulfurization on the activated rubber powder B, controlling the temperature of an air inlet medium to be 400 ℃ and the outlet temperature to be 200 ℃, allowing the flash evaporation passage time to be 1min to obtain desulfurized rubber powder C, performing conventional plastication on the desulfurized rubber powder C, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging the obtained product to obtain regenerated rubber D.
Example 5
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 1.2: 4: 0.1 mixing and emulsifying, and further mixing with water according to the weight ratio of 1:3 to form a stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the weight ratio of the waste rubber particles to the solution A is 1: 10, collecting rubber powder of 40 meshes, and centrifugally removing liquid to obtain activated rubber powder B with 15% of liquid content;
the waste rubber particles are tire tread vulcanized rubber full tire particles, and the particle size is 10 meshes;
(3) and (3) performing flash evaporation desulfurization on the activated rubber powder B, controlling the temperature of an air inlet medium to be 420 ℃ and the outlet temperature to be 210 ℃, passing through a flash evaporation passage for 1.5min to obtain desulfurized rubber powder C, performing conventional plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging to obtain regenerated rubber D.
Example 6
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 0.8: 2.5: 0.3, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:9 to form a stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the weight ratio of the waste rubber particles to the solution A is 1: 6, collecting 60-mesh rubber powder, and centrifugally removing liquid to obtain activated rubber powder B with the liquid content of 10%;
the waste rubber particles are tire tread vulcanized rubber full tire particles, and the particle size is 10 meshes;
(3) and (3) performing flash evaporation desulfurization on the activated rubber powder B, controlling the temperature of an air inlet medium to be 380 ℃ and the outlet temperature to be 190 ℃, allowing the flash evaporation passage time to be 1min to obtain desulfurized rubber powder C, performing conventional mechanical plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging the sheet to obtain regenerated rubber D.
Comparative example 1
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 1: 3: 0.2, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:4 to form a stable solution A;
(2) the method comprises the following steps of carrying out wet cutting and grinding on waste rubber particles by adopting a solution A, wherein the waste rubber particles are tire tread vulcanized rubber full tire particles, the particle size is 5 meshes, and the weight ratio of the waste rubber particles to the solution A is 1: 8, collecting rubber powder of 40 meshes, and centrifugally removing liquid to obtain activated rubber powder B with 15% of liquid content;
(3) putting the activated rubber powder B into a vertical type stirring devulcanizer for desulfuration, wherein the desulfuration conditions are as follows: keeping the temperature at 225 ℃ and the pressure at 2.3MPa for 0.5h, then carrying out conventional plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging the sheet to obtain the reclaimed rubber.
Comparative example 2
A production method of high-performance environment-friendly reclaimed rubber comprises the following steps:
(1) selecting palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 1: 3: 0.2, mixing and emulsifying to form a stable solution A;
(2) the method comprises the following steps of conventionally crushing waste rubber particles (tire tread vulcanized rubber full-tire particles) into 30 meshes, then putting the particles into a vertical desulfurization tank with stirring, and then adding a solution A, an activating agent and warm water at 80 ℃, wherein the weight ratio of the waste rubber particles to the solution A to the activating agent to the warm water is 1: 0.15: 0.0005: 0.1, introducing steam into a jacket, keeping the steam pressure at 0.9-0.98MPa, stirring for 3h, finally performing conventional plastication, controlling the plastication temperature to be less than or equal to 60 ℃, and discharging to obtain the regenerated rubber.
The properties of the reclaimed rubbers of examples 1 to 6 according to the present invention and comparative examples 1 to 2 were measured according to the general Specification for reclaimed rubbers (GB/T13460 to 2016), and the results are shown in Table 1.
TABLE 1 test results of the properties of reclaimed rubber of the present invention
As can be seen from Table 1, the reclaimed rubber obtained in the comparative example has significantly reduced tensile strength and elongation at break, increased Mooney viscosity ML (1 + 4) at 100 ℃ and significantly reduced performance in the comparative example 2 by conventional desulfurization in the comparative example 1 and conventional pulverization and conventional desulfurization in the comparative example 2 (prior art water-oil method).
The reclaimed rubber obtained in the embodiments 1-6 of the invention has Mooney viscosity ML (1 + 4) of 55-65 N.m at 100 ℃, tensile strength of 11.5-14.2MPa, elongation at break of 355-385 percent and excellent performance.
Claims (7)
1. The production method of the high-performance environment-friendly reclaimed rubber is characterized by comprising the following steps of:
(1) mixing palm oil, naphthenic oil, rosin and petroleum sodium sulfonate according to a weight ratio of 1: 0.8-1.2: 2.5-4: 0.1-0.3, mixing and emulsifying, and further mixing with water according to the weight ratio of 1:1-9 to form stable solution A;
(2) carrying out wet cutting and grinding on waste rubber particles by adopting the solution A, and removing liquid to obtain activated rubber powder B;
(3) and carrying out flash evaporation regeneration on the activated rubber powder B to obtain desulfurized rubber powder C, and plasticating to obtain regenerated rubber D.
2. The method for producing high-performance environment-friendly reclaimed rubber according to claim 1, wherein the waste rubber particles in the step (2) are tire tread vulcanized rubber whole tire particles, and the particle size is 5-10 meshes.
3. The method for producing high-performance environment-friendly reclaimed rubber according to claim 1, wherein the weight ratio of the waste rubber particles and the solution A in the step (2) is 1: 5- -10.
4. The method for producing the high-performance environment-friendly reclaimed rubber according to claim 1, wherein the particle size of the activated rubber powder B in the step (2) is 30-60 meshes.
5. The method for producing the high-performance environment-friendly reclaimed rubber according to claim 1, wherein the liquid content of the activated rubber powder B in the step (2) is 10-15%.
6. The method for producing high-performance environment-friendly reclaimed rubber according to claim 1, wherein the flash evaporation conditions in the step (3) are as follows: the air inlet temperature is 380 ℃ minus 420 ℃, the air outlet temperature is 190 ℃ minus 210 ℃, and the time for passing through the flash channel is 1-1.5 min.
7. The method for producing the high-performance environment-friendly reclaimed rubber according to claim 1, wherein the plastication temperature in the step (3) is less than or equal to 60 ℃.
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| EP4116336A1 (en) * | 2021-07-09 | 2023-01-11 | The Goodyear Tire & Rubber Company | Rubber product devulcanization method and product |
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