WO2012122727A1

WO2012122727A1 - Microwave continuous foaming plate of tire reclaimed rubber and preparation method thereof

Info

Publication number: WO2012122727A1
Application number: PCT/CN2011/073238
Authority: WO
Inventors: 潘民光
Original assignee: 佛山惠幅化工有限公司
Priority date: 2011-03-14
Filing date: 2011-04-25
Publication date: 2012-09-20
Also published as: CN102146175A; CN102146175B

Abstract

A microwave continuous foaming plate of tire reclaimed rubber is made from material which comprises reclaimed rubber, sulfur powder, zinc oxide, accelerating agent, paraffin, stearic acid, polyethylene glycol-4000, antioxidant, and foaming agent. The preparation method comprises the following steps: a. thinning reclaimed rubber material, then adding the processed rubber and aromatic oil in an open mill to mix; (b) adding paraffin, stearic acid and polyethylene glycol into the rubber in turn at 70-90 degree Celsius, and the processed rubber discharging, calendering at 110-130 degree Celsius, and then cooling, (c)adding sulfur powder, zinc oxide and other additives in the rubber in turn to mix, and then calendering. The processed rubber is foamed and vulcanized in a microwave hot air circulating oven. The plate is cheap, and good in performance. The preparation method which can be done continuously has high yield and low labor intensity.

Description

Tire reclaimed rubber microwave continuous foaming sheet and preparation method thereof

Technical field

The invention relates to the application of a reclaimed rubber, in particular to a foam produced by using reclaimed rubber and a preparation method thereof, and belongs to the technical field of utilization of reclaimed rubber.

Background technique

In the field of polymers, the application of foaming materials has become more extensive, such as polystyrene foam board, polyvinyl chloride foam insulation board, polyurethane foaming rubber and the like. Due to the porosity of the foamed material, it can absorb higher energy during the compression process, and thus is widely used in the fields of packaging, protection and the like. However, due to the defects in the preparation of some foam materials, such as the existence of environmental defects, the product can not achieve continuous production and other issues, the development of foam materials is limited.

For example, foamed polystyrene (EPS) used to be used for packaging. EPS is used as a snack box in China, but the material cannot be recycled after use, causing white pollution. It has been banned internationally; PVC (polyethylene) is A general-purpose plastic with better comprehensive physical properties, but PVC is harmful in the production process and PVC can form carcinogens. As the society became more and more environmentally friendly, improved and environmentally friendly foaming materials were produced, such as Chinese patents (publication number). CN 101215391 A) discloses a preparation method of a chlorinated polyethylene modified nitrile rubber foaming material for realizing environmentally-friendly and low-cost foaming material preparation; Chinese patent (announcement number CN 101392076 B) From the perspective of the continuity of the production process, a new preparation method of the neoprene foamed sheet is proposed. These new inventions have promoted the development of the industry to a certain extent. At present, the development of foaming materials is mainly concentrated on the development of raw materials and the continuity of production.

Recycled rubber refers to the rubber that can be re-vulcanized by the physical and chemical processes such as crushing, heating and mechanical treatment of the waste rubber, which can be re-vulcanized. It is also one of the rubber raw materials prepared by foaming materials.

China's reclaimed rubber has sufficient supply, low price, excellent aging resistance, and good physical and mechanical properties. In addition to replacing some raw rubber for rubber products, it can also be used to make some low-grade rubber products, which can not only reduce The cost of the product can also improve the production process, and at the same time, it can recycle the used tires and reduce the pollution of the used tires to the natural environment. In order to effectively use the reclaimed rubber, it is necessary to have a correct understanding of the characteristics and advantages and disadvantages of the reclaimed rubber, and then further processing according to the production needs to achieve its reuse. Recycled rubber has good plasticity, easy to mix with raw rubber and compounding agent, saving man-hours and reducing power consumption; small shrinkage, can make the product have smooth surface and accurate size; good fluidity, easy to make model products; anti-aging Good properties, can improve the natural aging resistance of rubber products; have good heat resistance, oil resistance, acid and alkali resistance. The vulcanization speed is fast and the scorch resistance is good. Due to the characteristics of the reclaimed rubber itself, its current main use is still limited to the rubber products industry. There are also some applications in other industries, but they are relatively few, and their application fields still need to be developed.

The preparation of recycled rubber into foaming material can greatly improve the utilization rate of recycled rubber. However, the foams prepared by using recycled rubber are mainly molded products, with low production efficiency, high labor intensity, and unstable production performance. The production capacity of continuous vulcanization foaming, therefore, it is of great significance to study a method for producing a foam material of reclaimed rubber with low production cost, good product performance and stable quality.

Summary of the invention

In view of the above deficiencies, the present invention provides a tire reclaimed rubber microwave continuous foaming sheet and a preparation method thereof, which utilizes reclaimed rubber and other auxiliary materials and auxiliary agents, and is subjected to processes such as plasticating, mixing, mixing, refining, microwave foaming, etc. In order to realize the preparation of the foamed sheet, the production cost is low, the product performance is excellent, the continuous production can be realized, the production efficiency is high, the output is large, and the labor intensity is low.

The technical solution adopted by the present invention is as follows:

The tire reclaimed rubber microwave continuous foaming sheet of the invention comprises the following materials in proportion by weight: 100 parts of reclaimed rubber, 1~2 parts of sulfur powder, 1~2 parts of zinc oxide of 99.7%, and 0.5~7 of accelerator Parts, paraffin wax 0.5~1 parts, stearic acid 1~2 parts, PEG-4000 1-2 parts, anti-aging agent 0.5~1 parts, foaming agent ADC 5~10 parts, foaming agent ACP-W 1-3 parts.

The above sulfur powder is a 200-500 mesh sulfur powder.

The above accelerator is one or more of the accelerator D, the accelerator M, the accelerator BZ, and the accelerator ZDC.

The preparation method of the invention comprises the following steps:

(1) Adjust the roll distance of No. 1 open mill to 0.3-0.9mm, put the reclaimed rubber compound into thin pass, punch the triangle bag, and thin pass 3-6 times;

(2) Adjusting the roll distance of the No. 1 open mill to 1-3 mm, and putting the rubber compound processed in the step (1) into a wrapping roll until the surface is smooth and free of bubbles, and the film is formed to obtain a film;

(3) The film obtained in step (2) is forcibly cooled to room temperature and parked for 24-30 hours;

(4) The film obtained by the step (3) is cooled to a certain ratio of the aromatic hydrocarbon oil, and is mixed into the No. 1 internal mixer to mix the reclaimed rubber with the extracted oil;

(5) When the temperature of the No. 1 internal mixer reaches 70-90 ° C, paraffin, stearic acid and polyethylene glycol are added in sequence to carry out pressure mixing;

(6) When the temperature of the No. 1 internal mixer rises to 110~130 °C, the rubber compound after pressurization and kneading is discharged, and it is cast on the No. 2 open mill to be rolled out, and forced to cool to room temperature, and parked 8~10 After hours, the reclaimed rubber masterbatch after cooling;

(7) After weighing the cooled reclaimed rubber masterbatch, put it into the No. 2 internal mixer for 5 to 10 minutes, then add the foaming agent ADC for 2 to 5 minutes, then add the sulfur powder in turn. Zinc oxide, accelerator, anti-aging agent RD and foaming agent ACP-W, pressure mixing for 2 to 5 minutes, and then discharging;

(8) The No. 2 mixer discharge rubber is cast onto the No. 3 open mill for rolling out the sheet. First, the No. 3 open mill 0.3-0.6mm small roller pitch is 2-4 times, and the triangle is 2-3. Then, adjust the roll distance of No. 3 open mill to 2-5mm, the rubber package roll, cut the triangle bag 3-4 times, let the rubber roll, then cut the rubber into a width of 130-160mm The strip is hung on the trailer and forced to cool to room temperature;

(9) feeding the cooled strip to the extruder, performing an extrusion molding process to obtain a semi-finished product;

(10) Transfer the extruded semi-finished product through the oven drive roller, and enter the microwave heating air circulation oven to vulcanize and foam to obtain the finished foamed sheet.

In the preparation step (4), the weight ratio of the film to the aromatic oil is 8-15 parts of oil extracted per 100 parts of the glue.

The forced cooling method of the film, the rubber compound and the rubber strip in the preparation steps (3), (6), and (8) is carried out using an industrial fan.

In the preparation step (9), the extruder temperature was set to 50 ° C for the head, 45 ° C for the fuselage, 30 ° C for the screw, and 40 ° C for the feed port.

In the preparation step (10), the temperature of the oven is set to be 120 to 130 ° C in the first zone, 140 to 150 ° C in the second zone, 160 to 170 ° C in the third zone, and 170 to 175 ° C in the fourth zone.

In the preparation step (10), the length of the microwave heating air circulation oven is 30 to 40 meters.

The beneficial effects of the present invention over the prior art are:

(1) The foam produced by continuous extrusion of microwave refining method using reclaimed rubber has high production efficiency, high output, low labor intensity and continuous production capacity.

(2) The regenerated rubber which has been desulfurized by microwave has excellent plasticity, is easy to be kneaded and does not stick to the rubber during mixing, and the process adjustment is simple and the product quality is stable.

(3) Overcoming the problem that the existing reclaimed rubber foam is unstable, does not foam, has poor product performance, unstable quality, and uneven dispersion of the compounding agent.

DRAWINGS

Figure 1 is a process flow diagram.

detailed description

The invention is further illustrated by the following examples, which are intended to illustrate the invention and not to limit the scope of the invention.

Example 1

The tire reclaimed rubber microwave continuous foamed sheet was prepared by the following process steps.

(1) Adjust the roll distance of No. 1 open mill to 0.3mm, put the reclaimed rubber compound into thin pass, punch the triangle bag, and thin the pass 4 times; then adjust the roll distance of No. 1 open mill to 3mm, and put it into the previous one. After the step processing, the rubber compound is coated with a roll, and the surface is smooth and free of bubbles, and the film is formed, and the film is obtained; the film is forcibly cooled to room temperature by an industrial fan, and parked for more than 24 hours;

(2) The cooled film and aromatic oil are mixed according to the ratio of 8 parts of aromatic oil per 100 parts of glue, and mixed into the No. 1 internal mixer to mix the reclaimed rubber and the aromatic oil; when the No. 1 internal mixer When the temperature reaches 80 ° C, 0.8 parts of paraffin, 1 part of stearic acid, and polyethylene glycol-4000 are sequentially added. One part is subjected to pressure mixing; when the temperature of the No. 1 internal mixer rises to 120 ° C, the rubber compound after pressurization and kneading is discharged, cast into a No. 2 open mill, and the sheet is rolled, and forced to cool to room temperature with an industrial fan. , after parking for more than 8 hours, the reclaimed rubber masterbatch after cooling;

(3) Weigh the reclaimed rubber masterbatch after cooling, and then press it into the No. 2 internal mixer for 6 minutes, then add the foaming agent ADC. Mixing 5 parts for 2 minutes, then adding 300 parts of 300 parts of sulfur powder, 1.2 parts of 99.7% of zinc oxide, 1 part of accelerator D, 1.5 parts of accelerator M, 1 part of accelerator BZ, accelerator ZDC 0.5 parts, 0.5 parts of anti-aging agent RD and 1.5 parts of foaming agent ACP-W, pressurized and kneaded for 2 minutes, and then discharged;

(4) The No. 2 mixer discharge rubber is thrown onto the No. 3 open mill for rolling out the sheet. First, the No. 3 open mill 0.3mm small roll pitch is thinned 4 times, and the triangle bag is used twice, then the No. 3 The roll distance of the open mill is adjusted to 2mm, the rubber material is wrapped in a roll, and the triangle bag is cut and cut 3 times, so that the rubber material is wrapped in a roll. Then, the rubber material is cut into a 150 mm wide rubber strip and hung on the hanging car, and the industrial fan is used. Forced cooling to room temperature;

(5) Feeding the cooled strip into the extruder, setting the extruder temperature to: 50 ° C for the head, 45 ° C for the fuselage, 30 ° C for the screw, 40 ° C for the feed port, and performing the extrusion molding process. Getting a semi-finished product

(6) The extruded semi-finished product is conveyed through the oven drive roller, and is vulcanized and foamed into a microwave heating air circulation oven with a length of 30 meters to obtain a finished foamed sheet. The oven temperature is set to be 120 ° C in the first zone. The second zone is 142 ° C, the third zone is 160 ° C, and the fourth zone is 170 ° C.

Example 2

(1) Adjust the roll distance of No.1 open mill to 0.7mm, put the reclaimed rubber compound into thin pass, punch the triangle package, and thin the pass 3 times; then adjust the roll distance of No.1 open mill to 2mm, put it into the previous one. After the step processing, the rubber compound is coated with a roll, and the surface is smooth and free of bubbles, and the film is formed, and the film is obtained; the film is forcibly cooled to room temperature by an industrial fan, and parked for more than 24 hours;

(2) The film after cooling and the aromatic oil are mixed according to the ratio of 12 parts of oil extracted per 100 parts of glue, and mixed into the No. 1 internal mixer to mix the reclaimed rubber and the aromatic oil; when the No. 1 internal mixer When the temperature reaches 70 ° C, 0.5 parts of paraffin, 0.5 parts of stearic acid, and polyethylene glycol-4000 are sequentially added. 1.5 parts were subjected to pressure mixing; when the temperature of No. 1 internal mixer was raised to 120 ° C, the rubber compound after pressurization and kneading was discharged, and it was cast on a No. 2 open mill to be rolled out, and forced to cool to room temperature with an industrial fan. , after parking for more than 10 hours, the reclaimed rubber masterbatch after cooling;

(3) Weigh the reclaimed rubber masterbatch after cooling, put it into the No. 2 internal mixer for 5 minutes, and then add the foaming agent ADC. Mixing 6.5 parts for 5 minutes, then adding 300 parts of 300 parts of sulfur powder, 1 part of 99.7% of zinc oxide, 1 part of accelerator D, 2 parts of accelerator, 1 part of accelerator BZ, promoter ZDC 0.8 parts, 0.5 parts of anti-aging agent RD and 1 part of foaming agent ACP-W, pressure mixed for 5 minutes, and then discharged;

(4) The No. 2 internal mixer discharge rubber is cast onto the No. 3 open mill to be rolled out, firstly with a No. 3 open mill 0.5mm small roll distance thin pass 2 times, a triangular package 3 times, then 3 The roll gap of the open mill is adjusted to 3mm, the rubber material is wrapped in a roll, and the triangle bag is cut and cut 3 times, so that the rubber material is wrapped in a roll. Then, the rubber material is cut into a width of 140 mm and the rubber strip is hung on the hanging car, and the industrial fan is used. Forced cooling to room temperature;

(6) The extruded semi-finished product is conveyed through the oven drive roller, and is vulcanized and foamed into a microwave heating air circulation oven with a length of 35 meters to obtain a finished foamed sheet. The oven temperature is set to be: 125 ° C in the first zone, The second zone is 145 ° C, the third zone is 165 ° C, and the fourth zone is 170 ° C.

Example 3

(1) Adjust the roll distance of No.1 open mill to 0.5mm, put the reclaimed rubber compound into thin pass, punch the triangle bag and thin pass 5 times; then adjust the roll distance of No.1 open mill to 2mm, put it into the previous one. After the step processing, the rubber compound is coated with a roll, and the surface is smooth and free of bubbles, and the film is formed, and the film is obtained; the film is forcibly cooled to room temperature by an industrial fan, and parked for 30 hours;

(2) The cooled film and aromatic oil are mixed according to the ratio of 10 parts of aromatic oil per 100 parts of glue, and mixed into the No. 1 internal mixer to mix the reclaimed rubber with the aromatic oil; when the No. 1 internal mixer When the temperature reaches 85 ° C, 0.5 parts of paraffin, 2 parts of stearic acid, and polyethylene glycol-4000 are sequentially added. One part is subjected to pressure mixing; when the temperature of the No. 1 internal mixer rises to 110 ° C, the rubber compound after pressurization and kneading is discharged, cast into a No. 2 open mill, and the sheet is rolled, and forced to cool to room temperature with an industrial fan. , after parking for more than 10 hours, the reclaimed rubber masterbatch after cooling;

(3) After the cooled reclaimed rubber masterbatch is weighed, it is put into the No. 2 internal mixer for pressure mixing for 8 minutes, and then the foaming agent ADC is added. 8 parts of mixing for 3 minutes, then add 300 parts of sulfur powder 2 parts, 99.7% of zinc oxide 1.8 parts, accelerator D 1.5 parts, accelerator M 1.2 parts, accelerator BZ 2 parts, accelerator ZDC 0.5 parts, 1 part of anti-aging agent RD and 3 parts of foaming agent ACP-W, pressure mixed for 3 minutes, and then discharged;

(4) The No. 2 mixer discharge rubber is thrown onto the No. 3 open mill for rolling out the sheet. First, the No. 3 open mill 0.4mm small roller pitch is thinned twice, and the triangle bag is used for 3 times, then the No. 3 The roll distance of the open mill is adjusted to 5mm, the rubber material is wrapped in a roller, and the triangle bag is cut and cut 4 times, so that the rubber material is wrapped in a roll. Then, the rubber material is cut into a width of 130 mm and the rubber strip is hung on the hanging car, and the industrial fan is used. Forced cooling to room temperature;

(6) The extruded semi-finished product is conveyed through the oven drive roller, and is vulcanized and foamed into a microwave heating air circulation oven with a length of 35 meters to obtain a finished foamed sheet. The oven temperature is set to be: 128 ° C in the first zone, The second zone is 140 ° C, the third zone is 168 ° C, and the fourth zone is 172 ° C.

Example 4

(1) Adjust the roll distance of No.1 open mill to 0.9mm, put the reclaimed rubber compound into thin pass, punch the triangle bag and thin pass 6 times; then adjust the roll distance of No.1 open mill to 3mm, put it into the previous one. After the step processing, the rubber compound is coated with a roll, and the surface is smooth and free of bubbles, and the film is formed, and the film is obtained; the film is forcibly cooled to room temperature by an industrial fan, and parked for 30 hours;

(2) The cooled film and aromatic oil are mixed according to the ratio of 15 parts of aromatic oil per 100 parts of glue, and mixed into the No. 1 internal mixer to mix the reclaimed rubber and the aromatic oil; when the No. 1 internal mixer When the temperature reaches 90 ° C, 1 part of paraffin, 1.5 parts of stearic acid, and polyethylene glycol-4000 are added in sequence. 2 parts were subjected to pressure mixing; when the temperature of the No. 1 internal mixer was raised to 130 ° C, the rubber compound after pressurization and kneading was discharged, cast into a No. 2 open mill, and the sheet was rolled, and forced to cool to room temperature with an industrial fan. , after parking for more than 10 hours, the reclaimed rubber masterbatch after cooling;

(3) After the cooled reclaimed rubber masterbatch is weighed, put it into the No. 2 internal mixer for pressure mixing for 10 minutes, and then add the foaming agent ADC. 10 parts of mixing for 5 minutes, then add 300 parts of 300 parts of sulfur powder, 2 parts of 99.7% of zinc oxide, 2 parts of accelerator D, 1.8 parts of accelerator M, 1.5 parts of accelerator BZ, accelerator ZDC 1 part, anti-aging agent RD 0.8 part and foaming agent ACP-W 2.5 parts, pressure mixing for 5 minutes, and then discharging;

(4) The No. 2 mixer discharge rubber is cast onto the No. 3 open mill for rolling out the sheet. First, the No. 3 open mill 0.6mm small roller pitch is thinned 3 times, the triangle package is 2 times, then the 3rd is The roll distance of the open mill is adjusted to 4mm, the rubber material is wrapped in a roller, and the triangle bag is cut and cut 4 times, so that the rubber material is wrapped in a roller. Then, the rubber material is cut into a strip with a width of 160 mm and hung on the hanging vehicle, and the industrial fan is used. Forced cooling to room temperature;

(6) The extruded semi-finished product is conveyed through the oven drive roller, and is vulcanized and foamed into a microwave heating air circulation oven with a length of 35 meters to obtain a finished foamed sheet, and the oven temperature is set to be: 130 ° C in the first zone, The second zone is 150 ° C, the third zone is 170 ° C, and the fourth zone is 175 ° C.

Claims

1. A tire reclaimed rubber microwave continuous foaming sheet and a preparation method thereof, wherein the foamed sheet is prepared by the following materials in parts by weight: 100 parts of reclaimed rubber, 1 to 2 parts of sulfur powder, and 99.7% of zinc oxide 1~2 Parts, accelerator D 1 to 2 parts, accelerator M 1 to 2 parts, accelerator BZ 1 to 2 parts, accelerator ZDC 0.5 to 1 part, paraffin 0.5 to 1 part, stearic acid 1 to 2 parts, polyethylene glycol-4000 1 ~2 parts, anti-aging agent 0.5~1 part, foaming agent ADC 5~10 parts, foaming agent ACP-W 1~3 parts.

2. A tire reclaimed rubber microwave continuous foaming sheet according to claim 1 and a preparation method thereof, wherein the sulfur powder is 200-500 mesh sulfur powder

3. The tire reclaimed rubber microwave continuous foaming sheet and the preparation method thereof according to claim 1, wherein the accelerator is one of the accelerator D, the accelerator M, the accelerator BZ, and the accelerator ZDC. Several.

4. The tire reclaimed rubber microwave continuous foaming sheet and the preparation method thereof according to claim 1, wherein the method for preparing the foamed sheet comprises the following steps:

5. The preparation method according to claim 4, wherein in the step (4), the weight ratio of the film to the extracted oil is 8-15 parts of aromatic oil per 100 parts of the glue.

6. The preparation method according to claim 4, characterized in that the forced cooling method of the film, the rubber compound and the rubber strip in the steps (3), (6) and (8) is carried out by using an industrial fan.

7. The preparation method according to claim 4, characterized in that in the step (9), the temperature of the extruder is set to: a machine head of 50 ° C, a fuselage of 45 ° C, a screw of 30 ° C, and a feed port of 40 ° C.

8. The preparation method according to claim 4, wherein in the step (10), the temperature of the oven is set to be 120 to 130 ° C in the first zone, 140 to 150 ° C in the second zone, and 160 to 160 in the third zone. 170 ° C, the fourth zone 170 ~ 175 ° C.

9. The preparation method according to claim 4, wherein in the step (10), the length of the microwave heating air circulation oven is 30 to 40 meters.