CN106188721A - A kind of preparation method of high intensity reclaimed rubber - Google Patents

A kind of preparation method of high intensity reclaimed rubber Download PDF

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Publication number
CN106188721A
CN106188721A CN201610734967.1A CN201610734967A CN106188721A CN 106188721 A CN106188721 A CN 106188721A CN 201610734967 A CN201610734967 A CN 201610734967A CN 106188721 A CN106188721 A CN 106188721A
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parts
rubber
banburying
reclaimed rubber
high intensity
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仇颖超
薛荣飞
徐越
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Compositions Of Macromolecular Compounds (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

The present invention relates to the preparation method of a kind of high intensity reclaimed rubber, belong to the preparing technical field of reclaimed rubber.The present invention is first by after discarded butadiene-styrene rubber pretreatment, carry out respectively plastifying, desulfurization and banburying, obtain the sizing material after banburying, again the sizing material after banburying is carried out mixing mill with materials such as activator, Oleum Ricini, vulcanizing agent, age resisters, obtain reclaimed rubber, after pulverizing, reclaimed rubber powder is carried out mixing with materials such as organobentonite, coupling agent and calcium stearates, mixing rear extruding pelletization, i.e. can get high intensity reclaimed rubber.High intensity reclaimed rubber hot strength prepared by the present invention is higher, and hot strength reaches more than 12.5MPa;Using discarded butadiene-styrene rubber is raw material, and garbage heavily recycles, and is conducive to protecting environment, it is achieved the recycling of resource, the most socioeconomic sustainable development.

Description

A kind of preparation method of high intensity reclaimed rubber
Technical field
The present invention relates to the preparation method of a kind of high intensity reclaimed rubber, belong to the preparing technical field of reclaimed rubber.
Background technology
The quantity of waste old material is only second to waste plastics, wherein automobile tire whole world year in spent high molecular material Learies is more than 1,000,000,000, and China is at 5000~60,000,000.The recycling of waste old is based on damaged tire, and other also wraps Including scrap rubber footwear and the inner tube of a tyre etc., the utilization of scrap rubber is conducive to protecting environment, it is achieved the recycling of resource, the most socioeconomic Sustainable development.The quantity of waste old material is only second to waste plastics, the wherein full generation of automobile tire in spent high molecular material Boundary's year learies is more than 1,000,000,000, and China is at 5000~60,000,000.The recycling of waste old based on damaged tire, other Also including scrap rubber footwear and the inner tube of a tyre etc., the utilization of scrap rubber is conducive to protecting environment, it is achieved the recycling of resource, is conducive to society's warp The sustainable development of Ji.
Rubber powder used by conventional regeneration glue is based on junked tire, and other also includes prepared by waste rubber shoe and the inner tube of a tyre etc. , in regenerative process, generally all add the softening agent coal tar of a large amount of black, oil extract etc., the reclaimed rubber tool of preparation Having very niff, bigger contaminative, possibly together with the most poisonous chemical substance making people carcinogenic, current developed country Limit the rubbers such as the tire containing these chemical substances to use.Conventional regeneration glue needs at height at present in regenerative process Temperature digester is carried out, is usually added into substantial amounts of water, need heated and stirred, clean, be dehydrated, the operation such as refine.Its equipment and work Sequence is more complicated, and investment is big.Conventional regeneration glue current regeneration technology time typically at about 4h, steam pressure at about 1MPa, Time is long, and efficiency is low.Additionally the physical and mechanical properties of conventional regeneration glue is poor, and hot strength is typically 3~14MPa, but mostly 7~8MPa.
Summary of the invention
The technical problem to be solved: poor for the reclaimed rubber mechanical performance produced at present, hot strength is low, The problem shortening its service life, the present invention, first by after discarded butadiene-styrene rubber pretreatment, carries out plastifying, desulfurization and close respectively Refining, obtains the sizing material after banburying, then is carried out by the materials such as the sizing material after banburying and activator, Oleum Ricini, vulcanizing agent, age resister Mixing mill, obtains reclaimed rubber, by materials such as reclaimed rubber powder and organobentonite, coupling agent and calcium stearates after pulverizing Carry out mixing, mixing rear extruding pelletization, i.e. can get high intensity reclaimed rubber.High intensity reclaimed rubber mechanical performance prepared by the present invention Good, hot strength is high, extends its service life.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
(1) weigh 600~800g and discard butadiene-styrene rubber, with tap water by shred into after clean for its surface clean a diameter of 0.8~ 1.2cm crumb, puts into crumb 1:5 in mass ratio after soaking 1~2h in mass fraction 3% hydrochloric acid solution, filters to obtain filter Slag, puts in baking oven, inputs in Plasticator, at 200~300 DEG C and 3~5MPa at a temperature of 100~120 DEG C after being dried 5~7h Under the conditions of plastify 30~40min, remove pressure after plasticizing, and reduce temperature to room temperature, the crumb after plasticizing is pulverized, crosses 80 ~100 mesh sieves, obtain rubber powder;
(2) above-mentioned rubber powder is put in ultrasonic generator, under the conditions of frequency is 55~60Hz and power is 550~650W Desulfurization 25~35min, obtains pre-devulcanized rubber powder;
(3) above-mentioned pre-devulcanized rubber powder is joined in the banbury being connected with outer circulation cooling water, control rotor speed 50 ~70r/min, banburying time 10~15min under room temperature condition, making discharge temperature of charge after banburying is 80~120 DEG C, obtains banburying After sizing material;
(4) count by weight, choose the sizing material after 100~120 parts of above-mentioned banburyings, 0.8~1.2 part of activator 420,5 respectively ~7 parts of Oleum Ricini, 5~7 parts of stearic acid, 8~12 parts of antioxidant 264s, 5~10 parts of sulfur, 3~5 parts of zinc oxide and 3~5 parts of mistakes BP, adds double roller open the sizing material after banburying, activator 420, Oleum Ricini, stearic acid, antioxidant 264 the most successively In refining machine, arranging roll spacing is 3~5mm, and mill to back roller is away from for adding sulfur, zinc oxide and benzoyl peroxide first behind 1~2mm Acyl, continuing mill to roll spacing is 0mm, then bottom sheet after thin logical 10~20 times, obtains reclaimed rubber;
(5) above-mentioned reclaimed rubber is put in rubber crusher and pulverize, cross 30~40 mesh sieves, obtain rubber grain, by weight Meter, choose respectively 80~90 parts of rubber grains, 5~7 parts of organobentonites, 3~5 parts of coupling agent KH-590,5~7 parts of aluminium oxidies, 5~10 parts of nano silicons, 1~3 part of Pulvis Talci, 2~4 parts of calcium stearates, 5~7 parts of cellulose acetate, 10~12 parts of stones Wax, puts in mixing roll mixing 2~3h, mixing after add in double screw extruder, extruding pelletization, i.e. can get high intensity regeneration Glue.
The hot strength of high intensity reclaimed rubber prepared by the present invention reaches more than 12.5MPa, and elongation at break reaches 570% Above, shore hardness is more than 55H.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the high intensity reclaimed rubber hot strength that prepared by the present invention is higher, and hot strength reaches more than 12.5MPa;
(2) the high intensity reclaimed rubber that prepared by the present invention uses discarded butadiene-styrene rubber to be raw material, and garbage heavily recycles, and is conducive to Protection environment, it is achieved the recycling of resource, the most socioeconomic sustainable development.
Detailed description of the invention
First weigh 600~800g and discard butadiene-styrene rubber, a diameter of by shredding into after clean for its surface clean with tap water 0.8~1.2cm crumb, puts into crumb 1:5 in mass ratio after soaking 1~2h in mass fraction 3% hydrochloric acid solution, filters Filtering residue, put in baking oven, be dried at a temperature of 100~120 DEG C after 5~7g and input in Plasticator, 200~300 DEG C and 3~ Plastify 30~40min under the conditions of 5MPa, after plasticizing, remove pressure, and reduce temperature to room temperature, the crumb after plasticizing is pulverized, Cross 80~100 mesh sieves, obtain rubber powder;Above-mentioned rubber powder is put in ultrasonic generator, is 55~60Hz and merit in frequency Rate is desulfurization 25~35min under the conditions of 550~650W, obtains pre-devulcanized rubber powder;Again above-mentioned pre-devulcanized rubber powder is added To be connected with outer circulation cooling water banbury in, control rotor speed 50~70r/min, under room temperature condition the banburying time 10~ 15min, making discharge temperature of charge after banburying is 80~120 DEG C, obtains the sizing material after banburying;Count by weight, choose 100 respectively ~sizing material after 120 parts of above-mentioned banburyings, 420,5~7 parts of Oleum Ricini of 0.8~1.2 part of activator, 5~7 parts of stearic acid, 8~12 parts Antioxidant 264,5~10 parts of sulfur, 3~5 parts of zinc oxide and 3~5 parts of benzoyl peroxides, first the most successively by the sizing material after banburying, Activator 420, Oleum Ricini, stearic acid, antioxidant 264 add in double roller mill, and arranging roll spacing is 3~5mm, and mill is to rear Roll spacing is to add sulfur, zinc oxide and benzoyl peroxide after 1~2mm, and continuing mill to roll spacing is 0, thinner logical 10~20 Secondary rear bottom sheet, obtains reclaimed rubber;Above-mentioned reclaimed rubber is put in rubber crusher and pulverize, cross 30~40 mesh sieves, obtain rubber Grain, counts by weight, choose respectively 80~90 parts of rubber grains, 5~7 parts of organobentonites, 3~5 parts of coupling agent KH-590, 5~7 parts of aluminium oxidies, 5~10 parts of nano silicons, 1~3 part of Pulvis Talci, 2~4 parts of calcium stearates, 5~7 parts of acetate fibers Element, 10~12 parts of paraffin, put in mixing roll mixing 2~3h, mixing after add in double screw extruder, extruding pelletization, Obtain high intensity reclaimed rubber.
Example 1
First weigh 800g and discard butadiene-styrene rubber, after clean for its surface clean, shred into the broken rubber of a diameter of 1.2cm with tap water Glue, puts into crumb 1:5 in mass ratio after soaking 2h in mass fraction 3% hydrochloric acid solution, filters to obtain filtering residue, put in baking oven, Input after being dried 7h at a temperature of 120 DEG C in Plasticator, under the conditions of 300 DEG C and 5MPa, plastify 40min, after plasticizing, remove pressure Power, and reduce temperature to room temperature, pulverizes the crumb after plasticizing, crosses 100 mesh sieves, obtain rubber powder;By above-mentioned rubber powder Put in ultrasonic generator, desulfurization 35min under the conditions of frequency is 60Hz and power is 650W, obtain pre-devulcanized rubber powder;Again Above-mentioned pre-devulcanized rubber powder is joined in the banbury being connected with outer circulation cooling water, control rotor speed in 70r/min, room Banburying time 15min under the conditions of temperature, making discharge temperature of charge after banburying is 120 DEG C, obtains the sizing material after banburying;By weight Meter, choose respectively the sizing material after 120 parts of above-mentioned banburyings, 420,7 parts of Oleum Ricini of 1.2 parts of activators, 7 parts of stearic acid, 12 parts anti-old 264,10 parts of sulfur of agent, 5 parts of zinc oxide and 5 parts of benzoyl peroxides, first successively by the sizing material after banburying, activator 420, Semen Ricini Oil, stearic acid, antioxidant 264 add in double roller mill, and arranging roll spacing is 5mm, and mill to back roller is away from for adding after 2mm Sulfur, zinc oxide and benzoyl peroxide, continuing mill to roll spacing is 0mm, then bottom sheet after thin logical 20 times, obtains reclaimed rubber;Will Above-mentioned reclaimed rubber is put in rubber crusher and is pulverized, and crosses 40 mesh sieves, obtains rubber grain, count by weight, choose 90 respectively Part rubber grain, 7 parts of organobentonites, 5 parts of coupling agent KH-590,7 parts of aluminium oxidies, 10 parts of nano silicons, 3 parts of Talcums Powder, 4 parts of calcium stearates, 7 parts of cellulose acetate, 12 parts of paraffin, put into mixing 3h in mixing roll, mixing after add twin-screw extrusion In machine, extruding pelletization, i.e. can get high intensity reclaimed rubber.After testing, the hot strength of the high intensity reclaimed rubber that prepared by the present invention Reaching 12.6MPa, elongation at break reaches 578%, and shore hardness is 56H.
Example 2
First weigh 600g and discard butadiene-styrene rubber, after clean for its surface clean, shred into the broken rubber of a diameter of 0.8cm with tap water Glue, puts into crumb 1:5 in mass ratio after soaking 1h in mass fraction 3% hydrochloric acid solution, filters to obtain filtering residue, put in baking oven, Input after being dried 5h at a temperature of 100 DEG C in Plasticator, under the conditions of 200 DEG C and 3MPa, plastify 30min, after plasticizing, remove pressure Power, and reduce temperature to room temperature, pulverizes the crumb after plasticizing, crosses 80 mesh sieves, obtain rubber powder;Above-mentioned rubber powder is put Enter in ultrasonic generator, desulfurization 25min under the conditions of frequency is 55Hz and power is 550W, obtain pre-devulcanized rubber powder;Again will Above-mentioned pre-devulcanized rubber powder joins in the banbury being connected with outer circulation cooling water, controls rotor speed in 50r/min, room temperature Under the conditions of banburying time 10min, making discharge temperature of charge after banburying is 80 DEG C, obtains the sizing material after banburying;Count by weight, point Do not choose the sizing material after 100 parts of above-mentioned banburyings, 420,5 parts of Oleum Ricini of 0.8 part of activator, 5 parts of stearic acid, 8 parts of antioxidant 264s, 5 Part sulfur, 3 parts of zinc oxide and 3 parts of benzoyl peroxides, first successively by the sizing material after banburying, activator 420, Oleum Ricini, tristearin Acid, antioxidant 264 add in double roller mill, and arranging roll spacing is 3mm, and mill to back roller is away from for adding sulfur, oxygen after 1mm Changing zinc and benzoyl peroxide, continuing mill to roll spacing is 0mm, then bottom sheet after thin logical 10 times, obtains reclaimed rubber;By above-mentioned regeneration Rubber is put in rubber crusher and is pulverized, and crosses 30 mesh sieves, obtains rubber grain, count by weight, choose 80 parts of rubber respectively Grain, 5 parts of organobentonites, 3 parts of coupling agent KH-590,5 parts of aluminium oxidies, 5 parts of nano silicons, 1 part of Pulvis Talci, 2 parts of tristearin Acid calcium, 5 parts of cellulose acetate, 10 parts of paraffin, put into mixing 2h in mixing roll, in mixing rear addition double screw extruder, and extrusion Pelletize, i.e. can get high intensity reclaimed rubber.After testing, the hot strength of the high intensity reclaimed rubber that prepared by the present invention reaches 13.5MPa, elongation at break reaches 585%, and shore hardness is 57H.
Example 3
First weigh 700g and discard butadiene-styrene rubber, after clean for its surface clean, shred into the broken rubber of a diameter of 0.9cm with tap water Glue, puts into crumb 1:5 in mass ratio after soaking 2h in mass fraction 3% hydrochloric acid solution, filters to obtain filtering residue, put in baking oven, Input after being dried 6h at a temperature of 110 DEG C in Plasticator, under the conditions of 250 DEG C and 4MPa, plastify 35min, after plasticizing, remove pressure Power, and reduce temperature to room temperature, pulverizes the crumb after plasticizing, crosses 90 mesh sieves, obtain rubber powder;Above-mentioned rubber powder is put Enter in ultrasonic generator, desulfurization 30min under the conditions of frequency is 57Hz and power is 600W, obtain pre-devulcanized rubber powder;Again will Above-mentioned pre-devulcanized rubber powder joins in the banbury being connected with outer circulation cooling water, controls rotor speed in 60r/min, room temperature Under the conditions of banburying time 12min, making discharge temperature of charge after banburying is 90 DEG C, obtains the sizing material after banburying;Count by weight, point Do not choose the sizing material after 110 parts of above-mentioned banburyings, 420,6 parts of Oleum Ricini of 0.9 part of activator, 6 parts of stearic acid, 10 parts of antioxidant 264s, 7 parts of sulfur, 4 parts of zinc oxide and 4 parts of benzoyl peroxides, first successively by the sizing material after banburying, activator 420, Oleum Ricini, tristearin Acid, antioxidant 264 add in double roller mill, and arranging roll spacing is 4mm, and mill to back roller is away from for adding sulfur, oxygen after 1mm Changing zinc and benzoyl peroxide, continuing mill to roll spacing is 0mm, then bottom sheet after thin logical 15 times, obtains reclaimed rubber;By above-mentioned regeneration Rubber is put in rubber crusher and is pulverized, and crosses 35 mesh sieves, obtains rubber grain, count by weight, choose 85 parts of rubber respectively Grain, 6 parts of organobentonites, 4 parts of coupling agent KH-590,6 parts of aluminium oxidies, 7 parts of nano silicons, 2 parts of Pulvis Talci, 3 parts of tristearin Acid calcium, 6 parts of cellulose acetate, 11 parts of paraffin, put into mixing 2h in mixing roll, in mixing rear addition double screw extruder, and extrusion Pelletize, i.e. can get high intensity reclaimed rubber.After testing, the hot strength of the high intensity reclaimed rubber that prepared by the present invention reaches 14.5MPa, elongation at break reaches 575%, and shore hardness is 58H.

Claims (1)

1. the preparation method of a high intensity reclaimed rubber, it is characterised in that concrete preparation process is:
(1) weigh 600~800g and discard butadiene-styrene rubber, with tap water by shred into after clean for its surface clean a diameter of 0.8~ 1.2cm crumb, puts into crumb 1:5 in mass ratio after soaking 1~2h in mass fraction 3% hydrochloric acid solution, filters to obtain filter Slag, puts in baking oven, inputs in Plasticator, at 200~300 DEG C and 3~5MPa at a temperature of 100~120 DEG C after being dried 5~7h Under the conditions of plastify 30~40min, remove pressure after plasticizing, and reduce temperature to room temperature, the crumb after plasticizing is pulverized, crosses 80 ~100 mesh sieves, obtain rubber powder;
(2) above-mentioned rubber powder is put in ultrasonic generator, under the conditions of frequency is 55~60Hz and power is 550~650W Desulfurization 25~35min, obtains pre-devulcanized rubber powder;
(3) above-mentioned pre-devulcanized rubber powder is joined in the banbury being connected with outer circulation cooling water, control rotor speed 50 ~70r/min, banburying time 10~15min under room temperature condition, making discharge temperature of charge after banburying is 80~120 DEG C, obtains banburying After sizing material;
(4) count by weight, choose the sizing material after 100~120 parts of above-mentioned banburyings, 0.8~1.2 part of activator 420,5 respectively ~7 parts of Oleum Ricini, 5~7 parts of stearic acid, 8~12 parts of antioxidant 264s, 5~10 parts of sulfur, 3~5 parts of zinc oxide and 3~5 parts of mistakes BP, adds double roller open the sizing material after banburying, activator 420, Oleum Ricini, stearic acid, antioxidant 264 the most successively In refining machine, arranging roll spacing is 3~5mm, and mill to back roller is away from for adding sulfur, zinc oxide and benzoyl peroxide first behind 1~2mm Acyl, continuing mill to roll spacing is 0mm, then bottom sheet after thin logical 10~20 times, obtains reclaimed rubber;
(5) above-mentioned reclaimed rubber is put in rubber crusher and pulverize, cross 30~40 mesh sieves, obtain rubber grain, by weight Meter, choose respectively 80~90 parts of rubber grains, 5~7 parts of organobentonites, 3~5 parts of coupling agent KH-590,5~7 parts of aluminium oxidies, 5~10 parts of nano silicons, 1~3 part of Pulvis Talci, 2~4 parts of calcium stearates, 5~7 parts of cellulose acetate, 10~12 parts of stones Wax, puts in mixing roll mixing 2~3h, mixing after add in double screw extruder, extruding pelletization, i.e. can get high intensity regeneration Glue.
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CN107417964A (en) * 2017-06-19 2017-12-01 西藏加速工场孵化器有限公司 Production method for reclaimed rubber
CN108250523A (en) * 2017-12-18 2018-07-06 黄燕 Production method for reclaimed rubber
CN108250556A (en) * 2018-01-18 2018-07-06 厦门市金汤橡塑有限公司 A kind of method that overlap waste recovery utilizes
CN114055671A (en) * 2021-11-20 2022-02-18 湖南涟漪设计有限公司 Method for recycling color rubber material
CN114957825A (en) * 2022-07-12 2022-08-30 四川省隆昌海燕橡胶有限公司 Preparation process for producing engineering inner tube reclaimed rubber by using waste rubber

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Publication number Priority date Publication date Assignee Title
CN107417964A (en) * 2017-06-19 2017-12-01 西藏加速工场孵化器有限公司 Production method for reclaimed rubber
CN107417964B (en) * 2017-06-19 2021-06-01 浙江宏达橡胶股份有限公司 Preparation method of reclaimed rubber
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CN114055671A (en) * 2021-11-20 2022-02-18 湖南涟漪设计有限公司 Method for recycling color rubber material
CN114055671B (en) * 2021-11-20 2023-09-22 湖南涟漪设计有限公司 Recycling method of color rubber material
CN114957825A (en) * 2022-07-12 2022-08-30 四川省隆昌海燕橡胶有限公司 Preparation process for producing engineering inner tube reclaimed rubber by using waste rubber

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Application publication date: 20161207