CN114478840B - Functionalized reversion liquid rubber and preparation method thereof - Google Patents
Functionalized reversion liquid rubber and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
- C08C19/00—Chemical modification of rubber
- C08C19/30—Addition of a reagent which reacts with a hetero atom or a group containing hetero atoms of the macromolecule
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention relates to the field of waste rubber regeneration, and discloses a functionalized reversion liquid rubber and a preparation method thereof, wherein the functionalized reversion liquid rubber comprises the following raw materials in parts by weight: 100 parts of waste rubber powder, 0-20 parts of a softening agent and 1-30 parts of a composite functionalized modifier. The preparation method comprises the following steps: (1) crushing waste rubber to obtain waste rubber powder; (2) removing impurities in the waste rubber powder; (3) mixing the waste rubber powder, a softening agent and a composite functionalized modifier in proportion and then uniformly stirring; (4) and (3) feeding the uniformly stirred raw materials into a desulfurization extruder for extrusion desulfurization, and then grinding, filtering and cooling to obtain the functionalized reversion liquid rubber. The functional active group in the compound functionalized modifier is grafted to a reversion liquid rubber molecular chain, so that the final product of the functional modifier becomes liquid rubber which has an adhesive functional group, has the characteristic of a softening agent and can participate in vulcanization crosslinking of main rubber.
Description
Technical Field
The invention relates to the technical field of waste rubber regeneration, in particular to functionalized reversion liquid rubber and a preparation method thereof.
Background
With the rapid development of the automobile industry, the yield of waste tires is increased, and the global waste rubber is increased. Waste rubber belongs to industrial harmful waste, and is one of the most harmful garbage which can deteriorate natural environment, destroy vegetation growth, influence human health and endanger the ecological environment of the earth. The resource utilization of the waste rubber can relieve the shortage of rubber resources, protect the ecological environment, and take the way of circular economy, thereby having profound strategic significance.
The long-term dream of experts in recycling materials and rubber materials is a problem which is solved by recovering waste rubber tires or rubber products into recovered rubber or recovering the waste rubber tires or rubber products into liquid rubber and then returning the waste rubber tires or rubber products into the field of rubber materials, but the problems are limited by specialties, and although new technologies or new inventions are disclosed, few technologies which can actually achieve industrialization or meet requirements on material performance are provided. The invention discloses a method for producing liquid reclaimed rubber by using a screw extruder continuously, which is invented by professor Zhang Liqun of Beijing chemical university, and the like, and relates to a domestically-disclosed patent related to rubber regeneration technology, such as ' a method for producing liquid reclaimed rubber by using a screw extruder continuously, wherein the patent is invented by Beijing chemical university, Zhang Liqun et al, ' (patent application No. 201210069417.4), the invention discloses a technology for producing liquid reclaimed rubber by using a screw extruder continuously, and the invention utilizes a well-known traditional rubber regeneration mechanism, namely a method for breaking crosslinked disulfide bonds or polysulfide bonds in vulcanized rubber powder by using the characteristic that the polysulfide bonds in the vulcanized rubber powder are easier to break than carbon-carbon bonds, namely C-C ', and the crosslinked disulfide bonds in the vulcanized rubber are broken by means of the mechanical shearing force and higher temperature of the extruder, so that the vulcanized rubber with a reticular crosslinked structure is changed into flowable low-molecular rubber, and a softener and a desulfurizer are additionally added in the regeneration process, meanwhile, no functional group is introduced into the molecular structure of the final product, the product is actually a semi-cracked soft regenerated rubber, and the product can only be used for modifying asphalt and has poor adhesion and compatibility with a rubber matrix when being reused in a rubber material, so that the product is not beneficial to popularization and application.
Disclosure of Invention
The invention provides a functionalized reversion liquid rubber and a preparation method thereof, aiming at overcoming the problems of insufficient chemical properties and resource utilization disadvantage of the traditional regenerated liquid rubber.
In order to achieve the purpose, the invention adopts the following technical scheme:
a functionalized reversion liquid rubber comprises the following raw materials in parts by weight:
100 parts of waste rubber powder;
0 to 20 parts of a softener
1-30 parts of a composite functionalized modifier.
Preferably, the compound functionalized modifier comprises two or more compounds of 3-hydroxycyclopentene, hexadienoic acid, cyclooctadiene, cyclopentadiene, oligomeric pentadienoic acid and C9-C22 diene acid.
The invention adds compound functional modifier when the waste rubber is restored, the compound functional modifier includes the compound containing-C-and-COOH, -OH functional group, the-C-can click with-SH group produced by cracking waste rubber powder, the compound functional modifier is grafted to the molecular chain of the product, thus the product has-C-, COOH, -OH functional group, under the common action of all functional groups, the liquid rubber after the waste rubber is restored has good adhesive property and softening agent property, can be used as rubber processing auxiliary agent, and can participate in the vulcanization crosslinking of main rubber; meanwhile, the reversion liquid rubber obtained by the invention is ultra-low viscosity rubber, can be directly used as adhesive rubber, and has extremely wide application.
Preferably, the composite type functionalized modifier also comprises one or more of diphenyl disulfide, cyclopentadiene maleate and dicyclopentadiene maleate. Diphenyl disulfide, cyclopentadienylmaleate and dicyclopentadiene maleate are added into the compound functionalized modifier, so that the reaction of-C-and-SH can be catalyzed, functional groups are more easily grafted on a molecular chain of the reverted liquid rubber, and the performance of the reverted liquid rubber is improved.
Preferably, the particle size of the waste rubber powder is 5-80 meshes.
Preferably, the softener is one or more selected from liquid isoprene rubber, aromatic oil, vegetable oil, tall oil and pine tar.
The invention also discloses a preparation method of the functionalized reversion liquid rubber, which comprises the following steps:
(1) crushing waste rubber to obtain waste rubber powder;
(2) removing impurities in the waste rubber powder;
(3) mixing the waste rubber powder, a softening agent and a composite functionalized modifier in proportion and then uniformly stirring;
(4) and (3) feeding the uniformly stirred raw materials into a desulfurization extruder for extrusion desulfurization, and then grinding, filtering and cooling to obtain the functionalized reversion liquid rubber.
The principle of the invention is that the vulcanized rubber molecules of the three-dimensional net-shaped cross-linked structure are partially broken according to the expected requirement by utilizing the mechanochemical action generated by the mechanical shearing force when the extruder works and the energy generated by the high temperature of each heating section of the extruder to become flowable linear low-molecular rubber; meanwhile, under the chemical effects of high temperature and mechanical force, the double bonds in the molecules of the compound functionalized modifier and the sulfydryl in the molecules of the reversion liquid rubber are subjected to click chemical reaction, and further, functional active groups are grafted to the molecular chains of the reversion liquid rubber, so that the final product of the liquid rubber is the liquid rubber which has adhesive functional groups, has the characteristic of a softening agent and can participate in vulcanization crosslinking of the main rubber.
Preferably, the waste rubber in the step (1) is a waste rubber tire or vulcanized rubber product, and the waste rubber tire is selected from one or more of all-steel truck tires, passenger car tires, bias truck tires and light truck tires.
Preferably, in the step (3), the mixture is stirred at a high speed for 5-25 min at a temperature of 50-150 ℃ and then stirred at a low speed for 10-30 min at a temperature of 50-150 ℃, wherein the high-speed stirring speed is 50-600 rpm, and the low-speed stirring speed is 5-50 rpm.
Preferably, the desulfurization extruder in the step (4) is a single-screw, double-screw or three-screw extruder; the heating sections of the desulfurization extruder are not less than 4 zones, and the temperature of each heating section is controlled to be 100-480 ℃; the rotating speed of the desulfurization extruder is 5-100 rpm.
Preferably, each device is provided with a VOCs gas collecting and processing device in the preparation process. According to the invention, the VOCs gas collecting and treating devices are arranged on the devices, so that the pollution of VOCs volatilization to the environment in the preparation process of the recovered liquid rubber can be avoided, and the requirement of environmental protection in the production process is met.
Therefore, the invention has the following beneficial effects: the double bonds in the molecules of the compound functionalized modifier and the sulfydryl in the molecules of the reversion liquid rubber are subjected to click chemical reaction, and then functional active groups are grafted to the molecular chains of the reversion liquid rubber, so that the final product of the liquid rubber is the liquid rubber which has an adhesive functional group, has the characteristic of a softening agent and can participate in vulcanization crosslinking of main rubber.
Detailed Description
The invention is further described with reference to specific embodiments.
In the present invention, all the equipments and materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
General example:
a method for preparing a functionalized reversion liquid rubber, comprising the steps of:
(1) crushing the waste car tires to 5-80 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts by weight of waste rubber powder, 0-20 parts by weight of a softening agent and 1-30 parts by weight of a composite functionalized modifier; the compound functionalized modifier comprises two or more compounds of 3-hydroxycyclopentene, hexadienoic acid, cyclooctadiene, cyclopentadiene acid, oligomeric pentadienoic acid and C9-C22 dienoic acid; also comprises one or more of diphenyl disulfide, cyclopentadiene maleate and dicyclopentadiene maleate; the softener is selected from one or more of liquid isoprene rubber, aromatic oil, vegetable oil, tall oil and pine tar;
(4) conveying the mixed material in the step (3) to a high-speed stirrer, and stirring at a high speed for 5-25 min at a temperature of 50-150 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 50-600 rpm;
(5) conveying the materials in the step (4) to a pot, keeping the temperature at 50-150 ℃, and stirring at a low speed for 10-30 min at a rotating speed of 5-50 rpm;
(6) continuously feeding the material in the storage tank in the step (5) into a feed port of a desulfurization extruder to be extruded and desulfurized, and controlling the temperature of each heating section of the desulfurization extruder to be 100-480 ℃; the rotating speed of the desulfurization extruder is 5-100 rpm;
(7) transferring the liquid rubber subjected to desulfurization and extrusion in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Example 1:
a method for preparing a functionalized reversion liquid rubber, comprising the following steps:
(1) crushing the waste car tires to 20-40 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts by weight of waste rubber powder, 5 parts by weight of liquid isoprene rubber, 1 part by weight of hexadienoic acid, 1 part by weight of 1, 5-cyclooctadiene and 1 part by weight of diphenyl disulfide;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 20min at the temperature of 100 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 150 revolutions per minute;
(5) conveying the materials in the step (4) to a pot, keeping the temperature at 100 ℃, stirring at a low speed for 25min, and rotating at a speed of 20 r/min;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 10 heating sections of the double-screw desulfurization extruder are 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; the temperature is 200-300 ℃, the temperature is 200-250 ℃, and the rotating speed of the twin-screw desulfurization extruder is 65 revolutions per minute;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Example 2:
a method for preparing a functionalized reversion liquid rubber, comprising the following steps:
(1) crushing the waste car tires to 40 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts by weight of waste rubber powder, 1 part by weight of hexadienoic acid, 1 part by weight of 1, 5-cyclooctadiene, 2 parts by weight of C20-diene acid and 1 part by weight of cyclopentadiene maleate;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 20min at a temperature of 50 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 200 revolutions per minute;
(5) conveying the materials in the step (4) into a pot, keeping the temperature at 50 ℃, and stirring at a low speed for 25min at a rotating speed of 50 revolutions per minute;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 11 heating sections of the double-screw desulfurization extruder are respectively 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; the temperature is 250-370 ℃, 200-300 ℃, 200-250 ℃, and the rotating speed of the double-screw desulfurization extruder is 50 revolutions per minute;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reclaimed liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Example 3:
a method for preparing a functionalized reversion liquid rubber, comprising the steps of:
(1) crushing the waste car tires to 60 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts by weight of waste rubber powder, 1 part by weight of hexadienoic acid, 1 part by weight of cyclopentadiene acid, 3 parts by weight of 11, 14-eicosadienoic acid and 1 part by weight of dicyclopentadiene maleate;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 15min at the temperature of 110 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 150 revolutions per minute;
(5) conveying the materials in the step (4) to a pot, keeping the temperature at 110 ℃, stirring at a low speed for 20min, and rotating at a speed of 30 r/min;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 11 heating sections of the double-screw desulfurization extruder are respectively 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; the temperature is 250-370 ℃, 200-300 ℃, 200-250 ℃, and the rotating speed of the double-screw desulfurization extruder is 50 revolutions per minute;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Example 4:
(1) crushing the waste car tires to 20-40 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts of waste rubber powder, 5 parts of liquid isoprene rubber, 1 part of hexadienoic acid and 1 part of 1, 5-cyclooctadiene in parts by weight;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 20min at the temperature of 100 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 150 revolutions per minute;
(5) conveying the materials in the step (4) into a pot, keeping the temperature at 100 ℃, and stirring at a low speed for 25min at a rotating speed of 20 rpm;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 10 heating sections of the double-screw desulfurization extruder are respectively 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; the temperature is 200-300 ℃, the temperature is 200-250 ℃, and the rotating speed of the double-screw desulfurization extruder is 60 revolutions per minute;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Example 5:
a method for preparing a functionalized reversion liquid rubber, comprising the steps of:
(1) crushing the waste car tires to 20-40 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts by weight of waste rubber powder, 5 parts by weight of liquid isoprene rubber, 4 parts by weight of 3-hydroxycyclopentene, 10 parts by weight of hexadienoic acid and 1 part by weight of diphenyl disulfide;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 25min at the temperature of 100 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 150 revolutions per minute;
(5) conveying the materials in the step (4) into a pot, keeping the temperature at 100 ℃, and stirring at a low speed for 30min at a rotating speed of 30 rpm;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 10 heating sections of the double-screw desulfurization extruder are respectively 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; the temperature is 200-300 ℃, the temperature is 200-250 ℃, and the rotating speed of the double-screw desulfurization extruder is 70 r/min;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Comparative example 1:
a preparation method of a reversion liquid rubber comprises the following steps:
(1) crushing the waste car tires to 20-40 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts of waste rubber powder and 5 parts of tall oil in parts by weight;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 15min at the temperature of 110 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 150 revolutions per minute;
(5) conveying the materials in the step (4) into a pot, keeping the temperature at 110 ℃, and stirring at a low speed for 20min at a rotating speed of 30 revolutions per minute;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 11 heating sections of the double-screw extruder are respectively 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; 250-370 ℃, 200-300 ℃, 200-250 ℃ and 40 r/min of double-screw extruder rotation speed;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain a recovered liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
Comparative example 2:
a method for preparing a functionalized reversion liquid rubber, comprising the steps of:
(1) crushing the waste car tires to 20-40 meshes to obtain waste rubber powder;
(2) removing steel cords, fiber cords, metal impurities and inorganic impurities in the waste rubber powder in the step (1) by a physical method;
(3) mixing 100 parts by weight of waste rubber powder, 5 parts by weight of liquid isoprene rubber and 1 part by weight of 1, 5-cyclooctadiene;
(4) conveying the mixed material in the step (3) into a high-speed stirrer, and stirring at a high speed for 15min at the temperature of 110 ℃, wherein the rotating speed of the high-speed stirrer is as follows: 150 revolutions per minute;
(5) conveying the materials in the step (4) into a pot, keeping the temperature at 110 ℃, and stirring at a low speed for 20min at a rotating speed of 30 revolutions per minute;
(6) continuously feeding the materials in the storage tank in the step (5) into a feed port of a double-screw desulfurization extruder for extrusion, wherein the temperatures of 11 heating sections of the double-screw extruder are respectively 120-200 ℃, 200-250 ℃, 250-370 ℃ and 250-370 ℃; 250 to 370 ℃, 250 to 370 ℃ and 250 to 370 ℃; 250-370 ℃, 200-300 ℃, 200-250 ℃ and 40 r/min of double-screw extruder rotation speed;
(7) transferring the liquid rubber extruded in the step (6) into a cooling extruder, grinding, filtering, cooling, and finally discharging to obtain functionalized reversion liquid rubber;
(8) weighing, sampling, inspecting and packaging the reversion liquid rubber in the step (7);
(9) and (5) warehousing the qualified detected persons, and storing the unqualified persons alone for technical treatment.
The components of the reversion liquid rubbers obtained in the above examples and comparative examples were measured, and the results are shown in table 1.
Table 1: reversion liquid rubber component test results.
The reversion liquid rubbers prepared in the above examples and comparative examples were used as tackifiers for tire transition layer processing, and the performance profiles are shown in table 2 in comparison with the blank example using a commercially available tackifier (204 resin).
Table 2: and testing the performance of the tire transition layer.
As can be seen from tables 1 and 2, the reclaimed liquid rubber obtained by the method of the present invention in examples 1 to 5 has good adhesion and softening properties when used as a processing aid in tire processing, and can participate in vulcanization crosslinking of the main rubber. In addition, diphenyl disulfide is not added into the compound type functionalized modifier in the embodiment 4, and the compound type functionalized modifier has slight influence on the self-adhesiveness and the chemical adhesive force of rubber, so that the self-adhesiveness of rubber compound in the formula of the tire transition layer and the adhesive force between vulcanized rubber and a steel cord are reduced to some extent compared with the adhesive force in the embodiment 1; in example 5, although the addition ratio of the composite type functional modifier is large, the adhesive performance is not much different from that of the other examples, and the adhesion of the vulcanized rubber and the steel cord is even reduced compared with that of example 2. In contrast, in comparative example 1, a compound-type functionalized modifier is not added during the processing, and in comparative example 2, -COOH is not introduced into the molecular chain of the reconstituted liquid rubber, so that the adhesive property of the prepared reconstituted liquid rubber is obviously reduced compared with that in the examples.
Claims (8)
1. A functionalized reversion liquid rubber is characterized by comprising the following raw materials in parts by weight:
100 parts of waste rubber powder, namely waste rubber powder,
0 to 20 parts of a softening agent,
1-30 parts of a composite functionalized modifier;
the compound functionalized modifier comprises a compound of two or more than two of 3-hydroxycyclopentene, hexadienoic acid, 1, 5-cyclooctadiene, cyclopentadiene acid and docosadienoic acid;
the preparation method of the functionalized reversion liquid rubber comprises the following steps:
(1) crushing waste rubber to obtain waste rubber powder;
(2) removing impurities in the waste rubber powder;
(3) mixing the waste rubber powder, a softening agent and a composite functionalized modifier in proportion and then uniformly stirring;
(4) and (3) feeding the uniformly stirred raw materials into a desulfurization extruder for extrusion desulfurization, and then grinding, filtering and cooling to obtain the functionalized reversion liquid rubber.
2. A functionalized reversion liquid rubber according to claim 1, wherein the complex type functionalization modifier further comprises one or more of diphenyl disulfide, cyclopentadiene maleate, dicyclopentadiene maleate.
3. The functionalized reversion liquid rubber of claim 1, wherein the particle size of the waste rubber powder is 5-80 mesh.
4. The functionalized reversion liquid rubber of claim 1, wherein the softening agent is one or more selected from the group consisting of liquid isoprene rubber, aromatic oil, vegetable oil, tall oil and pine tar.
5. The functionalized recycled liquid rubber as claimed in claim 1, wherein the waste rubber in step (1) is a waste rubber tire or vulcanized rubber product, and the waste rubber tire is selected from one or more of all-steel truck tires, passenger car tires, bias truck tires and light truck tires.
6. The functionalized recycled liquid rubber as claimed in claim 1, wherein the stirring in step (3) is performed by high speed stirring at 50-150 ℃ for 5-25 min, and then low speed stirring at 50-150 ℃ for 10-30 min, wherein the high speed stirring speed is 50-600 rpm, and the low speed stirring speed is 5-50 rpm.
7. The functionalized reversion liquid rubber of claim 1, wherein the devulcanization extruder in step (4) is a single screw, twin screw or triple screw extruder; the heating sections of the desulfurization extruder are not less than 4 zones, and the temperature of each heating section is controlled to be 100-480 ℃; the rotating speed of the desulfurization extruder is 5-100 rpm.
8. A functionalized reversion liquid rubber according to claim 1, wherein each unit of the preparation process is provided with a VOCs gas collection and treatment unit.
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| CN107936331B (en) * | 2017-11-10 | 2020-10-02 | 北京化工大学 | Method for preparing regenerated rubber by continuous desulfurization of multi-stage screws |
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| 改性技术在轮胎再生胶中的应用;徐世传;《中国橡胶》;20190410(第04期);50-56 * |
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