CN1239660C - Granulating process for thiofide CBS and preparing method thereof - Google Patents

Granulating process for thiofide CBS and preparing method thereof Download PDF

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Publication number
CN1239660C
CN1239660C CN 200310115235 CN200310115235A CN1239660C CN 1239660 C CN1239660 C CN 1239660C CN 200310115235 CN200310115235 CN 200310115235 CN 200310115235 A CN200310115235 A CN 200310115235A CN 1239660 C CN1239660 C CN 1239660C
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China
Prior art keywords
cbs
granulation
dry
wet
water
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CN 200310115235
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CN1544565A (en
Inventor
梁斌
邓廷昌
刘忠海
曹耀强
柯长颢
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Lanzhou Chemical Industry Co china National Petroleum Corp
China National Petroleum Corp
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Lanzhou Chemical Industry Co china National Petroleum Corp
China National Petroleum Corp
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Abstract

The present invention relates to the new rubber vulcanization accelerator CBS granulation technology, and adopts composite polyvinyl acetate (EVA) aqueous latexes as adhesives. The adhesives have reasonable formulation and strong compatibility on different rubber, and residual components do not affect product performance at all. The present invention directly granulates wet materials (the moisture percentage is about 20%) centrifugally dewatered or dry materials (the moisture percentage is less than or equal to 1%) dried by airflow in the process of production by regulating the concentration of the adhesives. Dry accelerator CBS powder is added by 1 to 4% of total material input in the final stage of granulation in order to prevent particles in drying from adhesion and coalescence. The particles are dried in hot air of 70 to 100 DEGC. The particles are sieved after the heating loss of products reaches the index required by users, and are made into CBS particle finished products.

Description

Rubber vulcanizing accelerator CBS prilling process and equipment thereof
Technical field
The invention belongs to a kind of rubber vulcanizing accelerator CBS (chemical name: production technique N cyclohexyl 2 benzothiazole sulfenamide), specifically a kind of method and equipment thereof that wet-milling (about water ratio 20%) or dry powder rubber vulcanizing accelerator CBS is processed into granular product.
The powder of background technology rubber vulcanizing accelerator CBS have density little, easily fly upward, easily thermolysis particularly very easily adheres to the metallic surface, and itself be difficult for granulated characteristic under drying regime under wetting conditions.Powdery CBS has a large amount of dust from flying in producing and using, environmental problem is outstanding, and existing a lot of rubber production producer all requires to use granulated product.
Existing rubber vulcanizing accelerator CBS granulation production technique, it is the method that the latex extrusion about adding 20-30% becomes the CBS masterbatch in powdered CBS material, this method reduces the effective constituent of CBS, in use, because the compatibility problem between the latex that adds and the different rubber, require different uses that latex is done corresponding the adjustment, use very flexible so make the CBS product of masterbatch.In addition, the centrifuge dehydration wet feed (about water ratio 17~25%) in the production process must increase production cost through the drying process drying, and many primary dryings also can bring more or less influence to the inner quality of final CBS particulate product.
There is the shortcoming that operating environment is poor, the Granularity Distribution scope is big in the common pan-type pelletizer that generally uses in the CBS granulation process at present.
Summary of the invention
The object of the present invention is to provide a kind ofly fill a prescription rationally, strong and residual component does not influence product performance fully to the consistency of different rubber rubber vulcanizing accelerator CBS granulation binding agent.
Another object of the present invention is to provide a kind of directly centrifuge dehydration wet feed (about water ratio 20%) from production process or the siccative behind the air stream drying, and (water ratio<1%, production intensity is suitable, granulating rate is high, the method for the granular CBS product of good fluidity.
A further object of the present invention provides a kind of effective operating environment of improving, and the material mist that produces after the nozzle atomization is not outwards flown upward, the rubber vulcanizing accelerator CBS new exclusive Fitz chilsonator that the Granularity Distribution scope is dwindled.
Above-mentioned purpose is achieved through the following technical measures:
A kind of rubber vulcanizing accelerator CBS adhesive for granulating has adopted composite polyvinyl acetate (EVA) water-based latex as binding agent, and its chemical constitution is in parts by weight:
Vinyl acetate 90-110 part
Ethene 16-20 part
Polyvinyl alcohol (1788) 0.8-4 part
Emulsifying agent (OP-10) 2-6 part
Initiator (ammonium persulphate) 0.08-0.7 part
Sodium bicarbonate 0.1-0.6 part
Water 100-140 part
A kind of rubber vulcanizing accelerator CBS granulation novel process is characterized in that:
0.2-10% (mass percent) by the CBS dry material takes by weighing with above-mentioned binding agent, and water disperses as dispersion agent again, the water yield of adding with granulation after the water ratio of wet granular to reach 22-40% (wet basis) be standard;
In the CBS Fitz chilsonator, with the binder solution after disperseing with the air flow type jet nozzle atomizing after, evenly add in the CBS dry mash at the granulation operation initial stage; Or, directly use centrifuge dehydration wet feed granulation in the production process according to the concentration that the water ratio of wet granular after the water ratio of wet feed after the centrifuge dehydration in the production process and the granulation is regulated binder solution, can omit the drying process in the original production flow process;
From spray adding additives solution, went through 35-90 minute, particle can form and grow up to desired granularity, afterwards again to the dried CBS powder that wherein newly adds total approximately charging capacity 1-4%, make particle surface form drying layer, to prevent that particulate adheres to and coalescence in the drying;
Dry under 70-100 ℃ of hot blast at last, the product by heating decrement is sieved (generally speaking, the water content requirement of CBS finished granule≤1%) after reaching the desired index of user, gets the CBS finished granule.
A kind of rubber vulcanizing accelerator CBS new exclusive Fitz chilsonator has increased the fixed disk cover on the granulation dish; Macrobead accumulation area position is provided with high speed cutter in dish, and coupled motor is fixed on the disk cover of big grain accumulation area top.
Rubber vulcanizing accelerator CBS granulation novel process provided by the invention, surface chemistry at CBS, adopted composite polyvinyl acetate (EVA) water-based latex as binding agent first after the screening after deliberation, wherein contain a small amount of compound as linking agent, softening agent, initiator and defoamer such as polyvinyl alcohol, prescription is reasonable, stronger to the consistency of different rubber, and residual component does not influence product performance fully.This technology is by regulating the concentration of binding agent, can be directly from the wet mash granulation, thus omitting drying process in the original production flow process, the result can reduce product cost greatly, can also be because of lacking the inner quality that drying once improve product; Add the accelerator CBS dry powder of total approximately charging capacity 1-4% latter stage in the granulation operation, to prevent that particulate adheres to and coalescence in the drying, the CBS granular product dry afterwards, that screening obtains, intensity is suitable, size range is moderate, good fluidity, be easy to metering, quality product (intensity, particle diameter, weight loss on heating, ash, performance) meets technical indicator, satisfies customer requirements.This process using new exclusive tablets press carries out granulation to wet-milling (about water ratio 20%) or dry powder accelerator CBS, owing on the granulation dish, increased the fixed disk cover, the material mist that binder solution produces after by nozzle atomization during granulation does not outwards fly upward, and has effectively improved operator's labor condition; Exclusive high speed cutter has newly been designed in the appropriate location of macrobead accumulation area in dish, can Granularity Distribution is greatly improved excessive reunion grain fragmentation, has reduced the load of screening system.In addition, the easy M R of the structure of this Fitz chilsonator also is easy to dismounting and cleaning when a small amount of ramming material.
Description of drawings
Fig. 1 is the general flow chart of CBS granulation novel process of the present invention
Fig. 2 is the structure sectional view of the special-purpose Fitz chilsonator of the present invention
Fig. 3 is the vertical view of Fitz chilsonator
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail:
Embodiment 1: utilize dry powder to produce the CBS particulate product
Technical process as shown in Figure 1 takes by weighing CBS adhesive for granulating latex 63 grams that prepare in advance by subordinate list 1, in the hot water that the 449ml that adding is stirred is 70 ℃, treats to add in the header tank after binding agent is uniformly dispersed stand-by.Accelerator CBS dry mash 687 grams are added in the granulation dish; top cover closes; opening main drive motor makes the granulation dish with 28 rev/mins of rotations (generally in 10-30 rev/min of scope); open pressurized air simultaneously and binding agent header tank valve begins to spray adding additives; the control spray adds (generally in the 40-80ml/min scope) about flow 70ml/min; after having sprayed; start the granulation cutting knife; particle can form and grow up gradually; about 56 minutes (generally 38-60 minute scope in) back particle can reach desired granularity; again to the dry mash that wherein adds 14 grams; after treating that particle becomes the loose sphere of no conglomeration, stop all motors, open discharge hole for discharge; dry under 70-100 ℃ hot blast, get the CBS granulated product.
The chemical constitution table of table 1 CBS adhesive for granulating latex
Composition Weight
Vinyl acetate 90-110
Ethene 16-20
Polyvinyl alcohol (1788) 0.8-4
Emulsifying agent (OP-10) 2-6
Initiator (ammonium persulphate) 0.08-0.7
Sodium bicarbonate 0.1-0.6
Water 100-140
With method for sieving granulation product has been carried out particle size distribution analysis respectively, typical results sees Table 1:
The typical size distribution (siccative) of table 1 CBS granulation product
Size range, mm Weight, g Weight fraction, %
>2 372 50.08
2-0.9 171 23.36
0.9-0.41 103 14.07
<0.41 86 11.75
Add up to 732 100
Embodiment 2: utilize wet feed (about water ratio 20%) to produce the CBS particulate product
Technical process as shown in Figure 1 takes by weighing CBS adhesive for granulating latex 65 grams that prepare in advance by subordinate list 1, adds in 280ml70 ℃ the hot water that stirs, and treats to add in the header tank after binding agent is uniformly dispersed stand-by.With the accelerator CBS water ratio is that 20.47% wet mash, 890 grams add in the granulation dishes; top cover closes; opening main drive motor makes the granulation dish with 26 rev/mins of rotations (generally in 10-30 rev/min of scope); open pressurized air simultaneously and binding agent header tank valve begins to spray adding additives; the control spray adds flow 35ml/min (generally being controlled between 25-40ml/min); after having sprayed; start the granulation cutting knife; particle can form and grow up gradually; (generally 38-60 minute scope in) particle can reach desired granularity after about 50 minutes; again to the dry mash that wherein adds 15 grams; after treating that particle becomes the loose sphere of no conglomeration, stop all motors, open discharge hole for discharge; dry under 70-100 ℃ hot blast, get the CBS granulated product.
With method for sieving granulation product has been carried out particle size distribution analysis respectively, typical results sees Table 2:
The typical size distribution (siccative) of table 2 CBS granulation product
Size range, mm Weight, g Weight fraction, %
>3.5 144 19.49
2-3.5 386 52.23
<2 209 28.28
Add up to 739 100
As shown in Figure 2, the Fitz chilsonator that CBS granulation novel process provided by the invention is used is on the basis of original pan-type pelletizer, has increased fixed disk cover 2 on granulation dish 1; Exclusive high speed cutter 3 has newly been designed in the appropriate location of macrobead accumulation area in granulation dish 1, and coupled cutter motor 4 is fixed on the disk cover 2 of big grain accumulation area top, in addition, and among the figure: the 5-scraper; The 6-bearing; The 7-shaft coupling; 8-disk cover anchor.
The present invention has carried out ultimate compression strength and mixing application test to dried product:
Is that 20 CBS particles of 5mm are measured with the granule strength tester to mean diameter, and the average compressive resistance that records is about 7 newton.Can be scaled the ultimate compression strength 0.357Mpa (for the maximal projection area) of unit surface.Prove that through stacking simulated experiment particle does not have broken the generation under routine stacking condition.
In the mixing experimentation of standard rubbers, the CBS granulation product of the above-mentioned intensity that detects by an unaided eye and the mix situation of rubber raw material on the open type mixing roll are not observed seriously flying upward of being taken place when adding the powdery auxiliary agent in mixing process; Because the particle of producing be spherical, do not observe yet when adding the stearic acid particle, taken place advance to fly phenomenon, its required mixing time and in contrast the powdery auxiliary agent product of thing do not have significant difference.The standard mixing time of being tested is 15 minutes.
Accelerator CBS powder and granulated product have been carried out the control cure test,, then gained rubber plate-like product has been carried out the comparative experiments of tensile strength in standard cure condition (146 ℃, 30 minutes) sulfuration down.Test result shows all do not have significant difference with the breaking tenacity and the elongation limit of granular auxiliary agent sulfurized product and powdery contrast, and only three times of fixed length stretching intensity slightly descend, but still within limit of error.This point increases auxiliary dosage or prolongs curing time by a little and can both effectively be compensated.(test center of carbon black industrial research designing institute has submitted the control cure test report to)

Claims (2)

1, a kind of rubber vulcanizing accelerator CBS process for granulating is characterized in that:
Adopt composite polyvinyl acetate aqueous latex as binding agent, its chemical constitution is in parts by weight:
Vinyl acetate 90-110 part
Ethene 16-20 part
Polyvinyl alcohol 1788 0.8-4 parts
Emulsifier op-10 2-6 part
Initiator ammonium persulfate 0.08-0.7 part
Sodium bicarbonate 0.1-0.6 part
Water 100-140 part
Above-mentioned binding agent is taken by weighing by CBS dry material mass percent 0.2-10%, and water disperses as dispersion agent again, the water yield of adding with granulation after the water ratio wet basis of wet granular to reach 22-40% be standard;
In the CBS Fitz chilsonator, with the binder solution after disperseing with the air flow type jet nozzle atomizing after, evenly add in the CBS dry mash at the granulation operation initial stage; Or, directly use centrifuge dehydration wet feed granulation in the production process according to the concentration that the water ratio of wet granular after the water ratio of wet feed after the centrifuge dehydration in the production process and the granulation is regulated binder solution, can omit the drying process in the original production flow process;
From spray adding additives solution, went through 35-60 minute, particle can form and grow up to desired granularity, afterwards again to the dried CBS powder that wherein newly adds total charging capacity 1-4%, make particle surface form drying layer, to prevent that particulate adheres to and coalescence in the drying;
Dry under 70-100 ℃ of hot blast at last, the product by heating decrement is sieved after reaching the desired index of user, gets the CBS finished granule.
2, a kind of special-purpose Fitz chilsonator of the prilling process of rubber vulcanizing accelerator CBS according to claim 1 is characterized in that: Fitz chilsonator has increased fixed disk cover (2) on granulation dish (1); The macrobead accumulation area is provided with high speed cutter (3) in granulation dish (1), and coupled motor (4) is fixed on the disk cover (2) of big grain accumulation area top.
CN 200310115235 2003-11-24 2003-11-24 Granulating process for thiofide CBS and preparing method thereof Expired - Fee Related CN1239660C (en)

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Application Number Priority Date Filing Date Title
CN 200310115235 CN1239660C (en) 2003-11-24 2003-11-24 Granulating process for thiofide CBS and preparing method thereof

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CN1239660C true CN1239660C (en) 2006-02-01

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Publication number Priority date Publication date Assignee Title
CN101314699B (en) * 2008-07-16 2011-08-24 江苏黑松林粘合剂厂有限公司 Water-based adhesion agent and preparation thereof
CN104559123B (en) * 2014-12-30 2017-08-29 山东戴瑞克新材料有限公司 Rubber vulcanizing accelerator CBS granulation specialist additive, the preparation method of the additive and prilling process

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