CN1071116A - Production method of high-saturation regenerated rubber waterproof material - Google Patents

Production method of high-saturation regenerated rubber waterproof material Download PDF

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Publication number
CN1071116A
CN1071116A CN91109502A CN91109502A CN1071116A CN 1071116 A CN1071116 A CN 1071116A CN 91109502 A CN91109502 A CN 91109502A CN 91109502 A CN91109502 A CN 91109502A CN 1071116 A CN1071116 A CN 1071116A
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rubber
temperature
desulfurization
mixing
regenerated
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CN91109502A
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CN1037078C (en
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李光祖
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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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Abstract

A method for producing a high-saturation regenerated rubber waterproof material. The waste vulcanized rubber is used as main raw material, and the desulfurized waste vulcanized rubber is brominated or oxidized to prepare high-saturation regenerated rubber, then a small amount of raw rubber and compounding agent are added to chlorinate the natural rubber, so as to improve the ageing resistance of the natural rubber, and the regenerated rubber is further processed by the procedures of mixing, extrusion, calendering, vulcanization and the like to prepare various waterproof materials. The method has the advantages of low energy consumption, low cost, short production period, low investment and excellent aging resistance of products, and is a production method with great development prospect.

Description

Produciton method of waterproof high-saturation regenerated rubber material
The invention belongs to and a kind of waste or used vulcanized rubber is regenerated, be made into the method for various water-proof materials then.
Along with developing rapidly of construction industry, the waterproof of cement works roofing and underground project waterproof antiseepage are ubiquitous technical barriers, fail for a long time to be well solved always.Through continuous exploration and practice, developing and produce novel high polymer waterproof material has become direction, but up to now, all is that to adopt brand-new rubber be raw material, and cost height and the ageing resistance of product is poor can not adapt to the actual needs of construction industry.The renovation process that the inventor once proposed waste or used vulcanized rubber in 1987 (patent No. 87100611.1), and make water-proof material with the regenerated rubber after handling, obtained good effect, but also has the some shortcomings part, for example: this method need be pulverized waste or used vulcanized rubber, power consumption is big, and equipment is easy to wear, and desulfurization time is long etc.The present invention is to the improvement of above-mentioned patent and perfect.
The purpose of this invention is to provide a kind of is that main raw material, energy consumption are little with the waste or used vulcanized rubber, and cost is low, with short production cycle, less investment, no waste water and gas are polluted the production method of the water-proof material that the product ageing resistance is good.
The objective of the invention is to realize as follows:
The present invention is to be main raw material with the waste or used vulcanized rubber, and the waste or used vulcanized rubber after the desulfurization carried out the regenerated rubber that high saturation is made in bromination or chlorination, add then a spot of rubber (and to the prescription in natural rubber carry out chlorination, improve the ageing-resistant performance of caouttchouc) and Synergist S-421 95, again through mixing, prolong and press or extrude, vulcanize operations such as (compound coiled materials), thus regenerated rubber is made various water-proof materials.
Fig. 1 is a process flow diagram of the present invention.
Below in conjunction with accompanying drawing each master operation of the present invention and operating condition are described in detail.
1, the blob of viscose (not needing fragmentation) greater than 10 centimeters * 10 centimeters is classified, cleaned and be cut into to waste or used vulcanized rubber, in the desulfurizing machine of Horizontal band rotation, carry out dynamic desulfurization, desulfurization temperature 80-210 ℃, desulfurization time 30-50 minute, make regenerative agent with resin, the consumption of regenerative agent is per kilogram glue Piece 20-50 gram, the inside of desulfurizing machine are provided with one 3.5 kilowatts blower fan to hot cigarette purification depollution. Used resin is to go out pin oil behind the spices with ammonia leaf oil body, add colophonite and in distillation still, be heated to 280-320 ℃ after 4 hours, cooling is filtered and is made, its main component is: ammonia leaf pin oil 100, colophonite 80-90, useless transformer oil 50-70, formaldehyde (content 27% above 10-24, pentachlorothiophenol 3-8 NaOH 0.28-0.51.
2, bromination is processed, (activated carbon is inhaled the bromine amount: 3.04 gram molecule/grams) to make bromating agent with activated carbon suction bromine method, in common rubber mixing machine, desulfurization glue and bromating agent in 100: the ratio of 1.5-2 (weight ratio) batching, carrying out bromination processes, 15 minutes reaction time, reaction temperature 140-150 ℃.
3, chloridized, in common rubber mixing machine, desulfurization glue and bleaching smart (containing available chlorine 70%) in 100: the ratio of 3-3.9 (weight ratio) is prepared burden, and carries out chloridized, reaction times 15-20 minute, temperature of reaction 120-135 ℃.
Reclaimed rubber after bromination, the chlorination should detect, and must meet following physicals:
Tensile strength (MPa) 〉=11.5,300%, tensile modulus (MPa) 〉=4.2 is pulled apart elongation % 〉=420, and 100 ℃ * 5100h of thermooxidizing never degenerates.
4, rubber is handled, rubber (natural gum or synthetical glue) is dried under 70-80 ℃ temperature, time is 2-3 hour, the blob of viscose that is cut into 10cm * 10cm * 50cm is then plasticated, used plasticating equipment is XK-400 * 1000,60-80 ℃ of roller temperature, roller capacity 20-30 kilogram/car, time 5-7 branch/car, thin-pass number of times 10-13 time, roll spacing 0.3-0.5mm.Natural rubber in the prescription is improved the ageing-resistant performance of natural rubber, and its chlorination method is identical with the chlorination method of reclaimed rubber.
5, batching, with reclaimed rubber and rubber and the accurate weighing of handling of various Synergist S-421 95, specifically fill a prescription and be (unit: kilogram):
Reclaimed rubber 65 natural gums 9.2 synthetical glues 25.8
Carbon black 5 promotor (CZ) 0.18
Promotor (M) 0.15 promotor (TMTD) 0.10
Sulfur 1.2 stearic phenol 1.2 rosinols 1.8
Stearic acid 0.2 paraffin wax 0.1
Silicon oxide 0.7 antioxidant D 0.1 superfine active calcium 60
Fine particle calcium carbonate 30 active colloidal powders 20
6, mixing, with the compound mixing facilities (K450 * 1200) for preparing, 25.4 meters/minute of preliminary roller speed, speed ratio is 1: 1.27,60-70 ℃ of roller temperature, capacity 40-50 kilogram/car, time 30-40 minute, thin-pass roll spacing 0.3-0.5mm was put back roll spacing 8-12mm.Mixing even, thin-pass blanking, cooling sheet are down deposited anti-.Prolong as required and press or extrude.
7, extrude, extruding is sizing material under the screw rod extruding of extruding machine, by the shape of the mouth as one speaks block sequences of strip, makes the film quality even, dense.Used extruding machine specification is 115 * 870mm, five road hot water circulation temperature controls is arranged, water temperature 90-100 ℃.Screw speed 13-39/ branch, film maximum width 1370mm, film thickness 0.8-6mm, throughput 160-500Kg/h, thickness deviation ± 0.1mm, initiatively motor 18.5-55kw.
8, infrared heating sulfuration method is adopted in sulfuration, compound coiled material, and specification of equipment Heating temperature 142-160 ℃, vulcanizes with the dull and stereotyped sulphur machine of 13500 * 1200mm.
Film by above-mentioned operation is made can use ordinary method, prepares various waterproof rolls, coating, waterproof paint, and waterproofing unction exposes rubber item and reaches more than 100 kinds.
Production method provided by the invention has following advantage:
1, waste or used vulcanized rubber is not needed fragmentation and vulcanization process, simplified equipment, saved a large amount of power consumptions, thereby reduced production cost;
2, waste or used vulcanized rubber is adopted horizontal desulfurizing machine, dynamically desulfurization is a thermal source with far infrared rays, does not need to use steam heating, has shortened desulfurization time, has improved production efficiency effectively.
3, the sizing material through chlorination or bromination extrudes easily, and the expressing technique performance is improved significantly.
4, it is stronger that the sizing material that makes has an ozone proof, the cohesiveness height, and anti-good permeability, resistance to deterioration can reach outside the 30-50.
5, less investment, easily found the factory, with short production cycle, it is fast to recoup capital outlay, and saves the rubber consumption, to improving environmental pollution positive effect is arranged.
6, according to raw-material characteristics, prescription of the present invention has distinctive feature, utilize the water coolant of rubber mixing machine to be warmed to 90-100 ℃ through the batching of particular design, in establish five-way road room temperature vulcanization still, vulcanize, produce the sulfide type waterproof roll, save steam boiler and drum vulcanizer, can save 500 square metres in 1,200,000 yuan equipment and factory building.
Embodiment 1:
1, waste or used vulcanized rubber is classified, cleaned and be cut into the blob of viscose greater than 10 centimeters * 10 centimeters, 120 ℃ of desulfurization temperatures, the inside of desulfurizing machine is provided with one 3.5 kilowatts blower fan to hot cigarette purification depollution.Used resin is to go out pin oil behind the spices with ammonia leaf oil body, add colophonite and in still kettle, be heated to 300 ℃, after 4 hours, cooling is filtered and is made, and its main component is: ammonia leaf pin 100, colophonite 85, useless transformer oil 60, formaldehyde (content is more than 27%), five phenol reds 7, sodium hydroxide 0.35.
3, chloridized in common rubber mixing machine, is prepared burden desulfurization glue and bleaching smart (containing available chlorine 70%) in 100: 3.5 ratios (weight ratio), carry out chloridized, 17 minutes reaction times, 125 ℃ of temperature of reaction.
Reclaimed rubber after the bromination should detect, and must meet following physicals:
Tensile strength (MPa) 〉=11.5,300% tensile modulus (MPa) 〉=4.2 is pulled apart elongation % 〉=420, and 100 ℃ * 5100h of thermooxidizing never degenerates.
3, rubber is handled, rubber (natural gum or synthetical glue) is dried under 75 ℃ temperature, time is 2.5 hours, the blob of viscose that is cut into 10cm * 10cm * 50cm is then plasticated, used plasticating equipment is XK-400 * 1000,70 ℃ of roller temperature, 25 kilograms/car of roller capacity, time 5-7 branch/car, thin-pass number of times 10-13 time, roll spacing 0.3-0.5mm.Natural rubber in the prescription is carried out chlorination, improve the ageing-resistant performance of natural rubber, its chlorination method is identical with the chlorination method of reclaimed rubber.
4, batching, with reclaimed rubber and rubber and the accurate weighing of handling of various Synergist S-421 95, concrete prescription is: (unit: kilogram)
Reclaimed rubber 65 natural gums 9.2 synthetical glues 25.8
Carbon black 5 promotor (CZ) 0.18
Promotor (M) 0.15, promotor (TMTD) 0.10
Sulfur 1.2 stearic phenol 1.2 rosinols 8
Paraffin wax 0.1 silicon oxide 0.7 antioxidant D 1.0
Superfine active calcium 60 fine particle calcium carbonates 30 rubber powders 30
5, mixing, with the compound mixing facilities (KS450 * 1200) for preparing, 25.4 meters/minute of preliminary roller speed, speed ratio is 1: 1.27,65 ℃ of roller temperature, 45 kilograms/car of capacity, 35 minutes time, thin-pass roll spacing 0.4mm is put back roll spacing 10mm.Mixing even, thin-pass blanking, the following sheet of cooling are deposited anti-, prolong as required and press or extrude.
6, extrude, extrusion is a sizing material under the screw rod extruding of extruding machine, by the shape of the mouth as one speaks block sequences of strip, makes the film quality even, dense.Used extruding machine specification is 115 * 870mm, and five road hot water circulation temperature controls are arranged, and temperature is 95 ℃, screw speed 28/ minute, film maximum width 1370mm, film thickness 3mm, throughput 300Kg/h, thickness deviation ± 0.1mm, initiatively motor 40kw.
7, sulfuration, compound coiled material are to adopt infrared heating sulfuration method, 158 ℃ of temperature, and all the other adopt nature room temperature vulcanization method.
Embodiment 2:
Chloridized in common rubber mixing machine, is prepared burden desulfurization glue and bleaching smart (containing available chlorine 70%) in 100: 3.5 ratios (weight ratio), carry out chloridized, 17 minutes reaction times, 125 ℃ of temperature of reaction.
Reclaimed rubber after bromination, the chlorination should detect, and must meet following physicals:
Tensile strength (MPa) 〉=11.5,300% is stretched intensity (MPa) 〉=4.2, pulls apart elongation % 〉=420, and 100 ° * 5100h of thermooxidizing never degenerates.
All the other operations are with embodiment 1.

Claims (2)

1, a kind of production method of high saturation regenerated-rubber water-proofing material, it is characterized in that with waste or used vulcanized rubber for being main raw material, and the waste or used vulcanized rubber after the desulfurization carried out the regenerated rubber that high saturation is made in bromination or chlorination, add a spot of rubber and Synergist S-421 95 then, again through mixing, extrude, roll, operation such as sulfuration, thus regenerated rubber is made various water-proof materials, the operation sequence of employing is:
(1) blob of viscose (not needing fragmentation) greater than 10 centimeters * 10 centimeters is classified, cleaned and be cut into to waste or used vulcanized rubber, in the desulfurizing machine of horizontal band rotation, carry out dynamic desulfurization, desulfurization temperature 80-210 ℃, desulfurization time 30-50 minute, make regenerator with resin, the consumption of regenerator is a per kilogram blob of viscose 20-50 gram, and the inside of desulfurizing machine is provided with one 3.5 kilowatts blower fan to hot cigarette purification depollution.
(2) bromination is handled, with activated carbon inhale the bromine method make bromizating agent (activated carbon is inhaled the bromine amount: 3.04 mol/grams), in common rubber mixing machine, desulfurization glue and bromizating agent are prepared burden in the ratio (weight ratio) of 100:1.5-2, carry out bromination and handle 15 minutes reaction times, temperature of reaction 140-150 ℃
(3) chloridized in common rubber mixing machine, desulfurization glue and ratio (weight ratio) batching of bleaching smart (containing available chlorine 70%) in 100:3-3.9, is carried out chloridized, and reaction times 15-20 minute, temperature of reaction 120-135 ℃,
(4) rubber is handled, rubber (natural gum or synthetical glue) is dried under 70-80 ℃ temperature, time is 2-3 hour, the blob of viscose that is cut into 10cm * 10cm * 50cm is then plasticated, and used plasticating equipment is XK-400 * 400 * 1000,60-80 ℃ of roller temperature, roller capacity 20-30 kilogram/car, time 5-7 branch/car, thin-pass number of times 10-13 time, roll spacing 0.3-0.5mm
(5) batching, with reclaimed rubber and rubber and the accurate weighing of handling of various Synergist S-421 95, specifically fill a prescription and be (unit: kilogram):
Reclaimed rubber 65 natural gums 9.2 synthetical glues 25.8
Carbon black 5 promotor (CZ) 0.18
Promotor (M) 0.15, promotor (TMTD) 0.10
Sulfur 1.2 stearic phenol 1.2 rosinols 1.8
Stearic acid 0.2 paraffin wax 0.1
Silicon oxide 0.7 antioxidant D 0.1 superfine active calcium 60
Fine particle calcium carbonate 30 active colloidal powders 20
(6) mixing, with the compound mixing facilities (K450 * 1200) for preparing, 25.4 meters/minute of preliminary roller speed, speed ratio is 1: 1.27,60-70 ℃ of roller temperature, capacity 40-50 kilogram/car, time 30-40 minute, thin-pass roll spacing 0.3-0.5mm was put back roll spacing 8-12mm.It is mixing that evenly thin-pass blanking, the following sheet of cooling are deposited anti-,
(7) extrude, extruding is sizing material under the screw rod extruding of extruding machine, by the shape of the mouth as one speaks block sequences of strip, makes the film quality even, dense.Used extruding machine specification is 115 * 870mm, five road hot water circulation temperature controls is arranged, water temperature 90-100 ℃.Screw speed 13-39/ branch, film maximum width 1370mm, film thickness 0.8-6mm, throughput 160-500kg/, thickness deviation ± 0.2mm, active motor 18.5-55kw,
(8) infrared heating sulfuration method is adopted in sulfuration, compound coiled material, equipment used specification 13500 * 1200m/m, vulcanizing press, Heating temperature 142-160 ℃, vulcanize.
2, according to a kind of production method of claim 1, it is characterized in that used resin is to go out pin oil behind the spices with ammonia leaf oil body, add colophonite and in still kettle, be heated to 280-320 ℃ after 4 hours, cooling is filtered and is made, and its main component is: ammonia leaf pin oil 100, colophonite 80-90, useless transformer oil 50-70, formaldehyde (content is more than 27%) 10-24, pentachlorothiophenol 3-8, sodium hydroxide 0.28-0.51.
CN91109502A 1991-09-23 1991-09-23 Production method of high-saturation regenerated rubber waterproof material Expired - Fee Related CN1037078C (en)

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CN91109502A CN1037078C (en) 1991-09-23 1991-09-23 Production method of high-saturation regenerated rubber waterproof material

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Application Number Priority Date Filing Date Title
CN91109502A CN1037078C (en) 1991-09-23 1991-09-23 Production method of high-saturation regenerated rubber waterproof material

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CN1071116A true CN1071116A (en) 1993-04-21
CN1037078C CN1037078C (en) 1998-01-21

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996002372A1 (en) * 1994-07-15 1996-02-01 Forschungsstelle Dr. Kubsch Laboratorium Für Analytik, Radiometrie Und Umwelttechnologie Gmbh Method of reactivating used rubber particles or shredded rubber waste
CN1058031C (en) * 1995-11-28 2000-11-01 李光祖 Production method for low temp. liquid regenerated rubber
GB2358369A (en) * 1999-11-15 2001-07-25 Lee Dae Woo Method of manufacturing unvulcanised adhesive waterproof sheet
CN100513112C (en) * 2005-11-17 2009-07-15 深圳市格林美高新技术股份有限公司 Automobile and electronic waste rubber-plastic regenerative reuse process
CN104385232A (en) * 2014-09-28 2015-03-04 无锡市东北塘永丰橡塑厂 Production technology of handle for rubber hammer
CN104479054A (en) * 2014-12-25 2015-04-01 芜湖融汇化工有限公司 Chlorinated rubber and method for preparing chlorinated rubber from recovered desulfurized tire rubber

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996002372A1 (en) * 1994-07-15 1996-02-01 Forschungsstelle Dr. Kubsch Laboratorium Für Analytik, Radiometrie Und Umwelttechnologie Gmbh Method of reactivating used rubber particles or shredded rubber waste
CN1058031C (en) * 1995-11-28 2000-11-01 李光祖 Production method for low temp. liquid regenerated rubber
GB2358369A (en) * 1999-11-15 2001-07-25 Lee Dae Woo Method of manufacturing unvulcanised adhesive waterproof sheet
GB2358369B (en) * 1999-11-15 2004-04-21 Dae-Woo Lee A construction method using an unvulcanised waterproof sheet
US6890396B1 (en) 1999-11-15 2005-05-10 Lee Dae-Woo Method of manufacturing unvulcanized adhesive waterproof sheet and construction method using the same
CN100513112C (en) * 2005-11-17 2009-07-15 深圳市格林美高新技术股份有限公司 Automobile and electronic waste rubber-plastic regenerative reuse process
CN104385232A (en) * 2014-09-28 2015-03-04 无锡市东北塘永丰橡塑厂 Production technology of handle for rubber hammer
CN104479054A (en) * 2014-12-25 2015-04-01 芜湖融汇化工有限公司 Chlorinated rubber and method for preparing chlorinated rubber from recovered desulfurized tire rubber

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