CN1313522C - High-temperature continuous reproduction process of butyl rubber - Google Patents

High-temperature continuous reproduction process of butyl rubber Download PDF

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Publication number
CN1313522C
CN1313522C CNB200410066712XA CN200410066712A CN1313522C CN 1313522 C CN1313522 C CN 1313522C CN B200410066712X A CNB200410066712X A CN B200410066712XA CN 200410066712 A CN200410066712 A CN 200410066712A CN 1313522 C CN1313522 C CN 1313522C
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China
Prior art keywords
rubber
reacting
screw
cooling zone
butyl rubber
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CNB200410066712XA
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Chinese (zh)
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CN1754904A (en
Inventor
倪雪文
施兆丰
周洪
赵勇
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南通回力橡胶有限公司
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • 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
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/141Feedstock
    • Y02P20/143Feedstock the feedstock being recycled material, e.g. plastics
    • 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
    • Y02W30/70

Abstract

The present invention provides high-temperature continuous reproduction process for butyl rubber, which comprises the steps of raw material processing, grinding, batching, material feeding, desulphurization regenerating, refining, filtering, forming, etc., wherein softening agents and active agents are added according to proportion in the batching step; material is forcibly fed in the material feeding step; a purpose-made screw-rod desulphurization machine is used in the desulphurization regenerating step. A machine cavity of the screw-rod desulphurization machine in the present invention is orderly divided into seven heating reaction intervals and five cooling intervals, electric heating modules are respectively arranged in all the intervals, cooling devices are respectively arranged in all the cooling intervals, and the temperature of all the intervals is controlled in the prescribed range. Two screw rods are provided, and each screw rod has the structure that sectional spiral grooves with equal depth and unequal distance are combined with a sectional banburying engaging block and an inverse spiral groove. The high-temperature continuous reproduction process has the advantages of realization of continuous regeneration by using the process and the devices, stable product quality, no secondary pollution, and arbitrary regulation and selection of mooney values from 20 to 60 with the control range of +/-5, and meets the operation requirement of different users.

Description

High-temperature continuous reproduction process of butyl rubber

Technical field

The present invention relates to a kind of regeneration techniques and equipment of high molecular polymer waste material, particularly a kind of high-temperature continuous reproduction process of butyl rubber.

Background technology

Waste butyl rubber is a kind of rubber sources of preciousness, the annual waste butyl rubber that produces tens thousand of tons of China, and the isoprene-isobutylene rubber renovation process has mechanical process, chemical method, high temperature dynamic method, electronics speed irradiation method, enlightening to connect method of reproduction etc. both at home and abroad at present.Wherein mechanical process is to roll refining by machinery at normal temperatures to make the isoprene-isobutylene rubber molecular chain degradation, and this explained hereafter efficient is low, production cost height, of poor quality and superseded gradually.The characteristics of chemical method be with isoprene-isobutylene rubber under the effect of acid, alkali, molecular chain take place to destroy and reaches the regeneration purpose, is difficult to handle owing to produce a large amount of chemical residues in the production process, employee's operation is dangerous, this technology is eliminated at present.The characteristics of electron radiation method are under electronics speed irradiation its molecular chain to be degraded the rubber powder through freezing and pulverizing, and the butyl renewable rubber quality stability of production is relatively poor, and facility investment is big, and the production cost height does not enter suitability for industrialized production.

It is the most general to use high temperature dynamic method production butyl renewable rubber at present, its principle is the rubber powder that earlier the butyl waste Crumb rubber is broken into about 30 orders, pack into after stirring with a certain amount of tenderizer, activator, water then and be equipped with in the airtight digester of whipping appts, digester is by electricity or heat-conducting oil heating and increasing temperature and pressure, sizing material is molecular chain generation cracking under high temperature, high pressure, tenderizer effect, thereby reaches the regeneration purpose.Its regeneration condition is generally 210 ℃ of temperature, pressure 2.0Mpa, and 4 hours time, this technology exists shortcoming to mainly contain:

1. isoprene-isobutylene rubber is a kind of high temperature material, and dynamically the digester top temperature is 210 ℃, therefore causes the isoprene-isobutylene rubber molecular chain degradation not thorough, and the sizing material Mooney viscosity value is up to more than 60.

2. the isoprene-isobutylene rubber processibility of Sheng Chaning is relatively poor, and shrinking percentage is up to more than 30%.

3. produce large quantity of exhaust gas when sizing material goes out cylinder, cause secondary pollution.

4. whole technology interval type is produced, the quality instability, and staff labor intensity is big.

5. can not regenerating resin sulfurized isoprene-isobutylene rubber (the isoprene-isobutylene rubber resistance to elevated temperatures of resin cure is better, is not dynamically reacting in the digester).

Summary of the invention

The present invention is the problem that exists in the prior art isoprene-isobutylene rubber regeneration in order to solve, and a kind of high-temperature continuous reproduction process of butyl rubber that provides, and this technology can realize the cyclic regeneration of isoprene-isobutylene rubber, raises the efficiency, and can eliminate secondary pollution in the regenerative process.

The technical measures that the present invention takes are that a kind of high-temperature continuous reproduction process of butyl rubber is characterized in, may further comprise the steps:

A, raw materials pretreatment

To wipe out the non-butyl rubber composition as the waste butyl rubber of raw material, clean up then, and clean the back and surveyed, remove metallic impurity wherein with metal locator;

B, pulverizing

To pulverize with pulverizer through pretreated waste butyl rubber raw material, raw material adopts the open rubber breaker of a ditch one light to pulverize when being the sulfur vulcanization isoprene-isobutylene rubber, control rubber powder fineness is the 5-20 order, adopt high speed alloy emery wheel to pulverize when raw material is the resin cure isoprene-isobutylene rubber, control rubber powder fineness is less than 30 orders;

C, batching

The rubber powder that crushes is quantitatively sent into mixing tank by the material loading chain bucket, add activator and the tenderizer measure by proportioning then and stir;

D, feeding

Above-mentioned compound is assigned to the loading hopper of screw desulfurization machine by blanking device, sends into the pressure blanking device, by the machine chamber of forcing the blanking device feeding by the frequency conversion transfer roller;

E, desulfurization regeneration

Compound is promoted in the progressive process by screw rod in the machine chamber of screw desulfurization machine, and sizing material and under the effect of the shearing force that produces, is finished desulfurization regeneration when activator and tenderizer and screw rod promote to advance under 240 ℃~400 ℃ high temperature;

F, refining

After sizing material after the desulfurization comes out from screw desulfurization machine, directly send into refiner and carry out refining by e Foerderanlage;

G, filtration

Sizing material after the refining is sent into filter by conveyer and is filtered;

H, moulding

Sizing material after the filtration is shaped to block finished product with shaper.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, the proportioning weight of rubber powder described in the step c and tenderizer, activator is as follows:

When raw material is the sulfur vulcanization isoprene-isobutylene rubber, join tenderizer 1-4 part, activator 0.1-0.3 part by 100 parts of its rubber powders;

When raw material is the resin cure isoprene-isobutylene rubber, join tenderizer 3-8 part by 100 parts of its rubber powders.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, the tenderizer described in the step c is a paraffinic base rubber oil, described activator is a polyalkylbenzene phenol disulphide (420).

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, charging described in the step c, operation is automatically all carried out in the proportioning metering of activator and tenderizer and adding and stirring, its process is: rubber powder is sent into mixing tank by the material loading chain bucket, mixing tank places on the weighing transmitter, the material loading chain bucket stops feeding after the rubber powder that enters mixing tank reaches predetermined weight, tenderizer, the activator pump is opened metering automatically, pump cuts out automatically after reaching predetermined weight, tenderizer, magnetic valve below the activator case is opened automatically, the measured tenderizer activator of scale flows in the mixing tank, work as tenderizer, activator case weight peeling zero setting rear electromagnetic valve is closed automatically, mixing tank begins to stir, and stops behind the stirring certain hour, then by the certain time interval feed.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, the machine chamber of the screw desulfurization machine described in the step e is divided between interval and 5 cooling zones of 7 reacting by heating in proper order, the electrically heated module is housed respectively in each interval, refrigerating unit is housed respectively between each cooling zone, and the temperature control that each is interval within the limits prescribed.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, each interval temperature controlling range is as follows in the machine chamber of described screw desulfurization machine:

When raw material is the sulfur vulcanization isoprene-isobutylene rubber, first reacting by heating district: the 290-360 ℃, second reacting by heating district: the 290-360 ℃, the 3rd reacting by heating district: 290-360 ℃, the 4th reacting by heating district: 290-360 ℃, slender acanthopanax thermal reaction area: 290-360 ℃, the 6th reacting by heating district: 290-360 ℃, the 7th reacting by heating district: 260-330 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃;

When raw material is the resin cure isoprene-isobutylene rubber, first reacting by heating district: the 360-400 ℃, second reacting by heating district: the 360-400 ℃, the 3rd reacting by heating district: 360-400 ℃, the 4th reacting by heating district: 360-400 ℃, slender acanthopanax thermal reaction area: 360-400 ℃, the 6th reacting by heating district: 360-400 ℃, the 7th reacting by heating district: 260-330 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, the control of the engine speed of the screw desulfurization machine described in the step e is as follows: raw material is controlled at 150-250 rev/min when being the sulfur vulcanization isoprene-isobutylene rubber; Raw material is controlled at 200-300 rev/min when being the resin cure isoprene-isobutylene rubber.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, the roll spacing of the refiner described in the step f is less than 0.1mm.

Above-mentioned high-temperature continuous reproduction process of butyl rubber, wherein, the filter screen of the filter described in the step g is the 60-100 order.

A kind of screw desulfurization machine that is used for high-temperature continuous reproduction process of butyl rubber is characterized in, comprises support, is installed on the support and motor, reduction box and machine chamber that order links to each other and link to each other with reduction box and traverse the screw rod in machine chamber;

Described machine chamber is sequentially with between interval and 5 cooling zones of 7 reacting by heating, and the electrically heated module is housed respectively in each interval, refrigerating unit is housed between each cooling zone respectively, and the afterbody in machine chamber is provided with venting hole;

Deeply equidistant screw channels such as described screw rod is a twin screw, screw-rod structure employing segmentation and segmentation banburying interlock block and reverse screw channel are combined.

The present invention makes it compared with prior art owing to adopted above technical scheme, has following advantage and characteristics:

1, the present invention is according to the resistant to elevated temperatures characteristics of isoprene-isobutylene rubber, adopt continuous processing, high temperature (temperature is controlled at 240-400 ℃), normal pressure, hot oxygen, under shearing force and the tenderizer swelling action, make the C-S in the isoprene-isobutylene rubber, S-S chain or the rapid cracking of C-O-C key, in the machine chamber, promptly finish whole regenerative process, recovery time only is 10-15 minute, and effectively guaranteed the primary characteristic of isoprene-isobutylene rubber, the resistance to air loss of rubber, tensile strength and virgin rubber are consistent substantially, can arbitrarily transfer choosing between the Mooney point 20-60, span of control is ± 5, satisfies the service requirements of different user.

2, because rubber has certain elasticity and bonding agglomerating easily, if adopt common screw rod blanking device to carry out feeding, its speed is inhomogeneous, intermittently, sometimes rubber powder feeds not go down at all, therefore the present invention is ad hoc has counted one and has forced blanking device, hopper places on the frequency conversion transfer roller, its working face is very big, by the frequency conversion transfer roller rubber powder is delivered on the pressure blanking device, force the blanking device spiral darker, sizing material is fed screw desulfurization machine by force, guaranteed the homogeneity of sizing material feeding speed like this by high speed rotating.

3, sizing material will be brought the air of a part into the machine chamber in the forced feed process, machine cavity temperature height, and air is heated and expands, and causes sizing material to blow out when extruding easily like this, and product is discontinuous, influences the stability of quality product.Because the present invention is provided with venting hole on the machine chamber, the air of expanded by heating in the regenerative process can be discharged from venting hole, phenomenon such as stopped to blow out, two ends, machine chamber place under the normal pressure, have promoted the thermooxidizing of sizing material in the machine chamber.

4, isoprene-isobutylene rubber pulverizing characteristics are different from other rubber; sizing material is easy bonding conglomeration in rolling the refining process; be difficult for into powder; prior art is generally cut into slices with cutting machine or is used the plastic granulator granulation; or pulverize with cold method; all there is certain disadvantage in these methods, and dicing is unfavorable for the fast rapid regeneration of isoprene-isobutylene rubber, and cold method pulverizing cost is too high.The different characteristics of bound sulfur vulcanized butyl rubber of the present invention and resin cure isoprene-isobutylene rubber selects for use the open pulverizer of a ditch one light to pulverize the sulfur vulcanization isoprene-isobutylene rubber, and sizing material rolls and is smelt 5-20 order rubber powder and gets final product; The resin cure isoprene-isobutylene rubber selects for use high speed alloy emery wheel formula pulverizer to pulverize, and the rubber powder fineness reaches more than 30 orders, more than two kinds of specification rubber powders all can satisfy the desulfurization requirement.

5, since the screw desulfurization machine among the present invention the machine chamber is divided between interval and 5 cooling zones of 7 reacting by heating, independently electrically heated module is installed in each interval, control respectively by PC, between each cooling zone chilled water unit is installed, water coolant is controlled by magnetic valve, when temperature is higher than specified temperature, magnetic valve on the water-cooled tube is opened automatically, the cooling of lowering the temperature, when temperature is lower than specified temperature, magnetic valve cuts out automatically, so just can guarantee that each interval temperature is controlled within the scope of regulation always.Temperature control descends from high to low gradually between the cooling zone, and the reclaimed rubber temperature of extruding is lower than 80 ℃, does not have hot gas, thereby has stopped environmental pollution.

6, the present invention is according to the characteristics of isobutene-diene rubber regeneration, adopt twin screw, deeply equidistantly screw channel and segmentation banburying interlock block and reverse screw channel are combined in screw-rod structure employing segmentations etc., by increasing the compression ratio of screw rod, guarantee that sizing material is subjected to enough shearings and friction in the machine chamber, promote the fast rapid regeneration of isoprene-isobutylene rubber.

7, the sizing material after the desulfurization directly carries out refining among the present invention, greatly reduce the regeneration power consumption, the refiner roll spacing is filtered by conveyer feeding filter behind the refiner initial refining less than 0.1mm during refining, filter screen is the 60-100 order, can guarantee that the isobutene-diene rubber regeneration resistance to air loss is unaffected.

Adopt the butyl renewable rubber quality index of explained hereafter of the present invention to surpass Japanese JIS K6313:1999 standard, its correlation data is as shown in table 1.

Table 1 Project ??JIS ??K6313:1999 Qualitative data with the product of technology of the present invention and device fabrication

Butyl renewable rubber Butyl inner tube of a tyre regenerated rubber Butyl capsule regenerated rubber Moisture (%) ??≤1.00 ??≤1.00 Ash content (%) ??≤15.00 ??≤8.00 ??≤8.00 Acetone extract (%) ??≤20.00 ??≤10.00 ??≤15.00 Tensile strength (MPa) ??≥6.86 ??≥8.0 ??≥8.00 Tensile yield (%) ??≥450 ??≥480 ??≥480 Mooney viscosity ML100 ℃/(1+4) ? ??≤80 ? ? ??45±5/35±5 ? ? ??45±5/35±5 ? Density (g/cm 3) ??≤1.20 ??≤1.20 ??≤1.20

Annotate: Japanese JIS K6313:1999 standard is not segmented butyl renewable rubber, the general designation butyl renewable rubber.

Description of drawings

Performance characteristic of the present invention further describes by following embodiment and accompanying drawing thereof.

Fig. 1 is the production scheme of technology of the present invention;

Fig. 2 is the structural representation of the screw desulfurization machine among the present invention.

Embodiment

High-temperature continuous reproduction process of butyl rubber among the present invention can be described as follows in conjunction with Fig. 1:

After waste butyl rubber 1 enters factory, personnel test by specialized staff inspection, wipe out non-butyl rubber compositions such as patch, clean with cleaning machine 2 then, impurity such as silt on the inner tube of a tyre are cleaned up, cleaned the back and surveyed, wiped out in the lump totally, handled the back and pulverize with pulverizer 4 if any metals such as inflating valve, iron nails with metal locator 3.According to the different characteristics of sulfur vulcanization isoprene-isobutylene rubber and resin cure isoprene-isobutylene rubber, select different breaking methods for use.The sulfur vulcanization isoprene-isobutylene rubber adopts the open pulverizer of a ditch one light to pulverize, and isoprene-isobutylene rubber is rolled be smelt the thick rubber powder of 5-20 order and get final product; The resin cure isoprene-isobutylene rubber adopts high speed alloy emery wheel to pulverize, and the rubber powder fineness is greater than 30 orders.The sizing material that crushes is sent into loading hopper 5 by automatic conveying device, and then carry chain bucket 6 to send into material mixer 7 by material loading, whole mixing tank places on the weighing transmitter 8, arriving a certain amount of back material loading carries chain bucket 6 to stop feeding automatically, tenderizer, the activator of 10 li in activator weighing case 9, tenderizer weighing case are imported material mixer 7 automatically then, stirred then 8 minutes, this a series of work is all finished automatically by PC control, and rubber powder and tenderizer, activator proportioning are as shown in table 2:

Table 2 The sulfur vulcanization isoprene-isobutylene rubber The resin cure isoprene-isobutylene rubber Sulfur vulcanization butyl rubber powder ??100 Resin cure butyl rubber powder ??100 Paraffinic base rubber oil ??1-4 Paraffinic base rubber oil ??3-8 Regeneration activator 420 ??0.1-0.3 Regeneration activator

The sizing material back that stirs is assigned to loading hopper 13 on the screw desulfurization machine 12 by blanking device 11, frequency conversion transfer roller 14 is housed under the loading hopper, sizing material is sent into pressure blanking device 15, sizing material is sent into the machine chamber of screw desulfurization machine 12 by forcing blanking device, sizing material is at high temperature, finish whole regenerative process under the shear action, sizing material enters the machine chamber from spout and only needs to come out 10-15 minute to discharge port, whole machine chamber is divided between interval and 5 cooling zones of 7 reacting by heating, the electrically heated module is equipped with in each interval respectively, temperature can be regulated control automatically, refrigerating unit is housed respectively between each cooling zone, cooling effect is played in control by the electromagnetism water valve, thereby guarantee that temperature is controlled within the scope of regulation, the concrete regeneration condition of butyl renewable rubber is as shown in table 3:

Table 3 Kind The reacting by heating district The first reacting by heating district The second reacting by heating district The 3rd reacting by heating district The 4th reacting by heating district The slender acanthopanax thermal reaction area The 6th reacting by heating district The 7th reacting by heating district The sulfur vulcanization isoprene-isobutylene rubber ? ??290-360 ? ??290-360 ? ??290-360 ? ??290-360 ? ??290-360 ? ??290-360 ? ??260-330 The resin cure isoprene-isobutylene rubber ? ??360-400 ? ??360-400 ? ??360-400 ? ??360-400 ? ??360-400 ? ??360-400 ? ??260-330

Table 3 (continuing) Kind The cooling zone Engine speed (r/min) First cooling zone Second cooling zone The 3rd cooling zone The 4th cooling zone The 5th cooling zone The sulfur vulcanization isoprene-isobutylene rubber ??180-200 ? ??120-180 ? ??80-120 ? ??60-80 ? ??60-80 ? ??150-250 ? The resin cure isoprene-isobutylene rubber ? ??180-200 ? ? ??120-180 ? ? ??80-120 ? ? ??60-80 ? ? ??60-80 ? ? ??200-300 ?

Sizing material after the desulfurization does not need kneading, directly send into refiner 16 and carry out refining by e Foerderanlage, the refiner roll spacing is 0.07-0.1mm, sizing material after the refining is sent sizing material into filter 18 by conveyer 17 and is filtered, filter screen is the 60-100 order, sizing material after the filtration promptly gets block finished product 20 with shaper 19 moulding after the weighing.21 is the tenderizer jar among the figure, and 22 is the activator jar.

Referring to Fig. 2, the screw desulfurization machine 12 among the present invention comprises pedestal 121, is installed on the pedestal and motor 122, reduction box 123 and machine chamber 124 that order links to each other and link to each other with reduction box and traverse the screw rod 125 in machine chamber.Machine chamber 124 is sequentially with between interval 1241 and 5 cooling zones of 7 reacting by heating 1242, and electrically heated module (not shown) is housed respectively in each interval, refrigerating unit (not shown) is housed, the venting hole 1243 that the afterbody in machine chamber is established respectively between each cooling zone.Deeply equidistant screw channels such as screw rod 125 is a twin screw, screw-rod structure employing segmentation and segmentation banburying interlock block and reverse screw channel are combined.

Further specify the present invention below in conjunction with embodiment.

Embodiment one

With the sulfur vulcanization isoprene-isobutylene rubber is raw material, pulverize with the open pulverizer of a ditch one light through after the pre-treatment, control rubber powder fineness is the 5-20 order, the rubber powder that crushes is quantitatively sent into mixing tank by the material loading chain bucket, and the proportioning that adds paraffinic base rubber oil 3 weight parts, polyalkylbenzene phenol disulphide (420) 0.2 weight parts by raw material 100 weight parts adds paraffinic base rubber oil and polyalkylbenzene phenol disulphide and stirs then; Then above-mentioned compound is assigned to the loading hopper of screw desulfurization machine by blanking device, send into the pressure blanking device by the frequency conversion transfer roller, carry out desulfurization regeneration by the machine chamber of forcing blanking device feeding screw desulfurization machine, as follows in each interval temperature control of regenerative process: first reacting by heating district: the 300-330 ℃, second reacting by heating district: the 300-330 ℃, the 3rd reacting by heating district: 300-330 ℃, the 4th reacting by heating district: 300-330 ℃, slender acanthopanax thermal reaction area: 300-330 ℃, the 6th reacting by heating district: 300-330 ℃, the 7th reacting by heating district: 240-280 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃; Engine speed is controlled at 150-200 rev/min.After sizing material after the desulfurization comes out from screw desulfurization machine, directly send into refiner and carry out refining by e Foerderanlage.Sizing material after the refining is sent into filter by conveyer and is filtered, and the filter screen of filter is selected 60 orders.Sizing material after the filtration is shaped to the block finished product of a kind of isobutene-diene rubber regeneration of the present invention with shaper.

Embodiment two

With the resin cure isoprene-isobutylene rubber is raw material, pulverizes with high speed alloy emery wheel through after the pre-treatment, and control rubber powder fineness is greater than 30 orders.The rubber powder that crushes is quantitatively sent into mixing tank by the material loading chain bucket, press raw material 100 weight parts then and add paraffinic base rubber oil 5 weight parts, and stir; Then above-mentioned compound is assigned to the loading hopper of screw desulfurization machine by blanking device, send into the pressure blanking device by the frequency conversion transfer roller, carry out desulfurization regeneration by the machine chamber of forcing blanking device feeding screw desulfurization machine, as follows in each interval temperature control of regenerative process: first reacting by heating district: the 370-390 ℃, second reacting by heating district: the 370-390 ℃, the 3rd reacting by heating district: 370-390 ℃, the 4th reacting by heating district: 370-390 ℃, slender acanthopanax thermal reaction area: 370-390 ℃, the 6th reacting by heating district: 370-390 ℃, the 7th reacting by heating district: 250-270 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃.Engine speed is controlled at 20-30 rev/min.After sizing material after the desulfurization comes out from screw desulfurization machine, directly send into refiner and carry out refining by e Foerderanlage.Sizing material after the refining is sent into filter by conveyer and is filtered, and the filter screen of filter is selected 90 orders.Sizing material after the filtration is shaped to the block finished product of a kind of isobutene-diene rubber regeneration of the present invention with shaper.

Embodiment three

With the sulfur vulcanization isoprene-isobutylene rubber is raw material, pulverize with the open pulverizer of a ditch one light through after the pre-treatment, control rubber powder fineness is the 5-20 order, the rubber powder that crushes is quantitatively sent into mixing tank by the material loading chain bucket, and the proportioning that adds paraffinic base rubber oil 4 weight parts, polyalkylbenzene phenol disulphide (420) 0.3 weight parts by raw material 100 weight parts adds paraffinic base rubber oil and polyalkylbenzene phenol disulphide and stirs then; Then above-mentioned compound is assigned to the loading hopper of screw desulfurization machine by blanking device, send into the pressure blanking device by the frequency conversion transfer roller, carry out desulfurization regeneration by the machine chamber of forcing blanking device feeding screw desulfurization machine, as follows in each interval temperature control of regenerative process: first reacting by heating district: the 320-350 ℃, second reacting by heating district: the 320-350 ℃, the 3rd reacting by heating district: 320-350 ℃, the 4th reacting by heating district: 320-350 ℃, slender acanthopanax thermal reaction area: 320-350 ℃, the 6th reacting by heating district: 320-350 ℃, the 7th reacting by heating district: 250-280 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃; Engine speed is controlled at 15-20 rev/min.After sizing material after the desulfurization comes out from screw desulfurization machine, directly send into refiner and carry out refining by e Foerderanlage.Sizing material after the refining is sent into filter by conveyer and is filtered, and the filter screen of filter is selected 80 orders.Sizing material after the filtration is shaped to the block finished product of a kind of isobutene-diene rubber regeneration of the present invention with shaper.

Embodiment four

With the resin cure isoprene-isobutylene rubber is raw material, pulverizes with high speed alloy emery wheel through after the pre-treatment, and control rubber powder fineness is greater than 30 orders.The rubber powder that crushes is quantitatively sent into mixing tank by the material loading chain bucket, press raw material 100 weight parts then and add paraffinic base rubber oil 8 weight parts, and stir; Then above-mentioned compound is assigned to the loading hopper of screw desulfurization machine by blanking device, send into the pressure blanking device by the frequency conversion transfer roller, carry out desulfurization regeneration by the machine chamber of forcing blanking device feeding screw desulfurization machine, as follows in each interval temperature control of regenerative process: first reacting by heating district: the 380-400 ℃, second reacting by heating district: the 380-400 ℃, the 3rd reacting by heating district: 380-400 ℃, the 4th reacting by heating district: 380-400 ℃, slender acanthopanax thermal reaction area: 380-400 ℃, the 6th reacting by heating district: 380-400 ℃, the 7th reacting by heating district: 260-330 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃.Engine speed is controlled at 20-30 rev/min.After sizing material after the desulfurization comes out from screw desulfurization machine, directly send into refiner and carry out refining by e Foerderanlage.Sizing material after the refining is sent into filter by conveyer and is filtered, and the filter screen of filter is selected 100 orders.Sizing material after the filtration is shaped to the block finished product of a kind of isobutene-diene rubber regeneration of the present invention with shaper.

Claims (10)

1. high-temperature continuous reproduction process of butyl rubber is characterized in that: may further comprise the steps:
A, raw materials pretreatment
To wipe out the non-butyl rubber composition as the waste butyl rubber of raw material, clean up then, and clean the back and surveyed, remove metallic impurity wherein with metal locator;
B, pulverizing
To pulverize with pulverizer through pretreated waste butyl rubber raw material, raw material adopts the open pulverizer of a ditch one light to pulverize when being the sulfur vulcanization isoprene-isobutylene rubber, control rubber powder fineness is the 5-20 order, adopt high speed alloy emery wheel to pulverize when raw material is the resin cure isoprene-isobutylene rubber, control rubber powder fineness is less than 30 orders;
C, batching
The rubber powder that crushes is quantitatively sent into mixing tank by the material loading chain bucket, add activator and the tenderizer measure by proportioning then and stir;
D, feeding
Above-mentioned compound is assigned to the loading hopper of screw desulfurization machine by blanking device, sends into the pressure blanking device, by the machine chamber of forcing blanking device feeding screw desulfurization machine by the frequency conversion transfer roller;
E, desulfurization regeneration
Compound is promoted in the progressive process by screw rod in the machine chamber of screw desulfurization machine, and sizing material and under the effect of the shearing force that produces, is finished desulfurization regeneration when activator and tenderizer and screw rod promote to advance under 240 ℃~400 ℃ high temperature;
F, refining
After sizing material after the desulfurization comes out from screw desulfurization machine, directly send into refiner and carry out refining by e Foerderanlage;
G, filtration
Sizing material after the refining is sent into filter by conveyer and is filtered;
H, moulding
Sizing material after the filtration is shaped to block finished product with shaper.
2. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1 is characterized in that: the proportioning weight of rubber powder described in the step c and tenderizer, activator is as follows:
When raw material is the sulfur vulcanization isoprene-isobutylene rubber, join tenderizer 1-4 part, activator 0.1-0.3 part by 100 parts of its rubber powders;
When raw material is the resin cure isoprene-isobutylene rubber, join tenderizer 3-8 part by 100 parts of its rubber powders.
3. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1 is characterized in that: the tenderizer described in the step c is a paraffinic base rubber oil, and described activator is a polyalkylbenzene phenol disulphide.
4. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1, it is characterized in that: the charging described in the step c, automatic red-tape operati is all carried out in the proportioning metering of activator and tenderizer and adding and stirring, its process is: rubber powder is sent into mixing tank by the material loading chain bucket, mixing tank places on the weighing transmitter, the material loading chain bucket stops feeding after the rubber powder that enters mixing tank reaches predetermined weight, tenderizer, the activator pump is opened metering automatically, pump cuts out automatically after reaching predetermined weight, tenderizer, magnetic valve below the activator case is opened automatically, the measured tenderizer activator of scale flows in the mixing tank, work as tenderizer, activator case weight peeling zero setting rear electromagnetic valve is closed automatically, mixing tank begins to stir, stop after stirring certain hour, then by the certain time interval feed.
5. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1, it is characterized in that: the machine chamber of the screw desulfurization machine described in the step e is divided between interval and 5 cooling zones of 7 reacting by heating in proper order, the electrically heated module is housed respectively in each interval, refrigerating unit is housed respectively between each cooling zone, and the temperature control that each is interval within the limits prescribed.
6. high-temperature continuous reproduction process of butyl rubber as claimed in claim 5 is characterized in that: each interval temperature controlling range is as follows in the machine chamber of described screw desulfurization machine:
When raw material is the sulfur vulcanization isoprene-isobutylene rubber, first reacting by heating district: the 290-360 ℃, second reacting by heating district: the 290-360 ℃, the 3rd reacting by heating district: 290-360 ℃, the 4th reacting by heating district: 290-360 ℃, slender acanthopanax thermal reaction area: 290-360 ℃, the 6th reacting by heating district: 290-360 ℃, the 7th reacting by heating district: 260-330 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃;
When raw material is the resin cure isoprene-isobutylene rubber, first reacting by heating district: the 360-400 ℃, second reacting by heating district: the 360-400 ℃, the 3rd reacting by heating district: 360-400 ℃, the 4th reacting by heating district: 360-400 ℃, slender acanthopanax thermal reaction area: 360-400 ℃, the 6th reacting by heating district: 360-400 ℃, the 7th reacting by heating district: 260-330 ℃, first cooling zone: 180-200 ℃, second cooling zone: 120-180 ℃, the 3rd cooling zone: 80-120 ℃, the 4th cooling zone: 60-80 ℃, the 5th cooling zone: 60-80 ℃.
7. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1 is characterized in that: the engine speed control of the screw desulfurization machine described in the step e is as follows: raw material is controlled at 150-250 rev/min when being the sulfur vulcanization isoprene-isobutylene rubber; Raw material is controlled at 200-300 rev/min when being the resin cure isoprene-isobutylene rubber.
8. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1 is characterized in that: the roll spacing of the refiner described in the step f is less than 0.1mm.
9. high-temperature continuous reproduction process of butyl rubber as claimed in claim 1 is characterized in that: the filter screen of the filter described in the step g is the 60-100 order.
10. screw desulfurization machine that is used for high-temperature continuous reproduction process of butyl rubber is characterized in that: comprise support, be installed on the support and motor, reduction box and machine chamber that order links to each other and link to each other with reduction box and traverse the screw rod in machine chamber;
Described machine chamber is sequentially with between interval and 5 cooling zones of 7 reacting by heating, and the electrically heated module is housed respectively in each interval, refrigerating unit is housed between each cooling zone respectively, and the afterbody in machine chamber is provided with venting hole;
Deeply equidistant screw channels such as described screw rod is a twin screw, screw-rod structure employing segmentation and segmentation banburying interlock block and reverse screw channel are combined.
CNB200410066712XA 2004-09-28 2004-09-28 High-temperature continuous reproduction process of butyl rubber CN1313522C (en)

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