CN107629489A - A kind of production method of modified carbon black - Google Patents
A kind of production method of modified carbon black Download PDFInfo
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- CN107629489A CN107629489A CN201710692914.2A CN201710692914A CN107629489A CN 107629489 A CN107629489 A CN 107629489A CN 201710692914 A CN201710692914 A CN 201710692914A CN 107629489 A CN107629489 A CN 107629489A
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Abstract
The present invention relates to rubber technical field, and in particular to supplies a kind of production method of modified carbon black.Carbon black is soaked 56 hours with concentration for 8 10% sulfuric acid, washed repeatedly with water to neutrality, soaked 1 1.5 hours with saturated sodium bicarbonate again, washed repeatedly with water to neutrality, carbon black after processing is calcined 30 40 minutes at 480 500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain modified carbon black, modification of the present invention need not change production of carbon black formula, the absorption iodine number of carbon black can be significantly reduced, improve the resistance tocrocking of carbon black, and the carbon black wearability after handling at least improves 35% compared with before processing, handling process is simple, equipment requirement is low, obtained black-reinforced performance is handled to effectively improve compared with before processing.
Description
Technical field
The present invention relates to rubber technical field, and in particular to supplies a kind of production method of modified carbon black.
Background technology
Carbon black is reinforcing filler important in reinforcing and filling system, and the physical and mechanical properties and processing technology to rubber size are all
Have a major impact, black particle diameter, structure and surface chemistries are the principal elements for determining carbon black property；In charcoal rubber weather strip often
Carbon black has N550, N762, N774, SP5000 etc., and this several carbon black has higher structure, medium reinforcing, extrudes work
The very property, and smooth in appearance that skill is become reconciled, all the time in occupation of leading position in EPDM sealing strip sizing compound formulas, in carbon black table
Face is generally contacted there is containing the impurity such as hydrogen, the functional group of oxygen and sulphur and tar, the oxide group in carbon black can pollute
Thing or working media, the extractives content in carbon black is higher, can migrate to product surface, cause surface blueing, it is general color the defects of,
Impurity content height can have a strong impact on the outward appearance and quality of basic product, such as occur age spot or cut etc. on surface, research
Show, carbon black iodine absorption number is bigger, and particle diameter is smaller, shows that specific surface area is bigger, and the more △ E numerical value of oxide group of carbon blacksurface are more
Height, obtained sealing strip resistance tocrocking is poorer, and therefore, the iodine absorption value for reducing carbon black has actively to improving carbon black resistance tocrocking
Meaning.
The content of the invention
It is an object of the invention to provide a kind of production method of modified carbon black.
The technical solution adopted by the present invention is a kind of production method of modified carbon black,
By carbon black with concentration be 8-10% sulfuric acid immersion 5-6 hours, washed repeatedly to neutrality with water, then soaked with saturated sodium bicarbonate
1-1.5 hours are steeped, are washed repeatedly to neutrality with water；
Carbon black after processing is calcined into 30-40 minutes at 480-500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain
To modified carbon black.
Preferably, it is that 8% sulfuric acid soaks 6 hours by carbon black concentration, is washed repeatedly to neutrality with water, then use unsaturated carbonate
Hydrogen sodium soaks 1.5 hours, is washed repeatedly to neutrality with water.
Preferably, it is that 10% sulfuric acid soaks 5 hours by carbon black concentration, is washed repeatedly to neutrality with water, then use unsaturated carbonate
Hydrogen sodium soaks 1 hour, is washed repeatedly to neutrality with water.
Preferably, the carbon black after processing is calcined 40 minutes at 480 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry in the air
It is dry, obtain modified carbon black.
Preferably, the carbon black after processing is calcined 30 minutes at 500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry in the air
It is dry, obtain modified carbon black.
Wherein, it is 8-10% sulfuric acid immersion 5-6 hours with concentration by carbon black, is washed repeatedly to neutrality with water, then use saturated carbon
Sour hydrogen sodium soaks 1-1.5 hours, is washed repeatedly with water to neutrality, carbon black is through immersing in sulfuric acid and saturated sodium bicarbonate solution
Afterwards, small material caused by reaction blocks carbon black micro channel, so as to reduce carbon black absorption iodine number, this anti-soil to improving carbon black
Metachromia has remarkable effect；
Wherein, the carbon black after processing is calcined into 30-40 minutes at 480-500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry in the air
It is dry, it is possible to increase carbon black hardness, and adhesive force and then the wearability for improving carbon black；
Modification of the present invention need not change production of carbon black formula, can significantly reduce the absorption iodine number of carbon black, improve the anti-of carbon black
Contaminative, and the carbon black wearability after processing at least improves 35% compared with before processing, handling process is simple, and equipment requirement is low, processing
Obtained black-reinforced performance effectively improves compared with before processing.
Embodiment
Embodiment 1：A kind of production method of modified carbon black, specific processing step are as follows：
It is that 8% sulfuric acid soaks 5 hours by carbon black concentration, is washed repeatedly to neutrality with water, then it is small with saturated sodium bicarbonate immersion 1
When, washed repeatedly to neutrality with water；
Carbon black after processing is calcined 30 minutes at 480 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
It is SP6000 carbon blacks as modification object to select kind, is divided into experimental group, control group 1, control group at random
2nd, totally 7 groups of control group 3, control group 4, control group 5, control group 6；
Experimental group is modified processing according to the mode of embodiment 1；
The cancellation step on the basis of embodiment 1 of control group 1（2）Carbon black is modified；
The cancellation step on the basis of embodiment 1 of control group 2（1）Carbon black is modified；
Control group 3 is cancelled concentration on the basis of embodiment 1 and carbon black was modified in 5 hours for the immersion of 8% sulfuric acid；
The cancellation on the basis of embodiment 1 of control group 4 is soaked 1 hour with saturated sodium bicarbonate to be modified to carbon black；
The carbon black on the basis of embodiment 1 of control group 5 is calcined to be substituted for for 30 minutes at 480 DEG C calcines carbon black at 470 DEG C
Carbon black was modified in 30 minutes；
The carbon black on the basis of embodiment 1 of control group 6 is calcined to be substituted for for 30 minutes at 480 DEG C calcines carbon black at 520 DEG C
Carbon black was modified in 30 minutes；
Iodine absorption value and wear-resisting value after each group modification are detected, and calculates wearability and improves ratio, wearability improves ratio
Calculation formula is：（The wear-resisting value of modified wear-resisting value-before modified）/ wear-resisting value before modified, as a result see the table below 1：
| Group | Experimental group | Control group 1 | Control group 2 | Control group 3 | Control group 4 | Control group 5 | Control group 6 |
| Iodine absorption value（mg/g） | 15.8 | 15.5 | 21.3 | 18.4 | 17.7 | 15.6 | 15.9 |
| Wearability improves ratio（%） | 36.8 | -2.2 | 39.5 | 39.9 | 40.2 | -1.8 | -1.3 |
As shown in Table 1, it is that 8% sulfuric acid soaks 5 hours by carbon black concentration, is washed repeatedly to neutrality with water, then with unsaturated carbonate hydrogen
Sodium soaks 1 hour, is washed repeatedly to neutrality with water；It is best to reducing carbon black iodine absorption number effect, and it is 8% arbitrarily to cancel with concentration
Sulfuric acid soaks 5 hours or soaked 1 hour with saturated sodium bicarbonate acts on equal unobvious to reducing carbon black iodine absorption number, after processing
Carbon black calcined 30 minutes at 480 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, have significantly to improving carbon black wearability
Effect, but arbitrarily reduction or increasing calcining temperature, then can not necessarily play and improve carbon black wearability effect, or even can reduce charcoal
Black wearability.
Embodiment 2：A kind of production method of modified carbon black, specific processing step are as follows：
It is that 8.2% sulfuric acid soaks 5.3 hours by carbon black concentration, is washed repeatedly to neutrality with water, then soaked with saturated sodium bicarbonate
1.1 hours, washed repeatedly to neutrality with water；
Carbon black after processing is calcined 32 minutes at 485 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
It is SP5000 carbon blacks as modification object to select kind, is divided into experimental group, control group 1, control group at random
2nd, totally 7 groups of control group 3, control group 4, control group 5, control group 6；
Experimental group is modified processing according to the mode of embodiment 2；
The cancellation step on the basis of embodiment 2 of control group 1（2）Carbon black is modified；
The cancellation step on the basis of embodiment 2 of control group 2（1）Carbon black is modified；
Control group 3 is cancelled concentration on the basis of embodiment 2 and carbon black was modified in 5 hours for the immersion of 8% sulfuric acid；
The cancellation on the basis of embodiment 2 of control group 4 is soaked 1 hour with saturated sodium bicarbonate to be modified to carbon black；
The carbon black on the basis of embodiment 2 of control group 5 is calcined to be substituted for for 32 minutes at 485 DEG C calcines carbon black at 470 DEG C
Carbon black was modified in 32 minutes；
The carbon black on the basis of embodiment 2 of control group 6 is calcined to be substituted for for 32 minutes at 485 DEG C calcines carbon black at 520 DEG C
Carbon black was modified in 32 minutes；
Iodine absorption value and wear-resisting value after each group modification are detected, and calculates wearability and improves ratio, wearability improves ratio
Calculation formula is：（The wear-resisting value of modified wear-resisting value-before modified）/ wear-resisting value before modified, as a result see the table below 2：
| Group | Experimental group | Control group 1 | Control group 2 | Control group 3 | Control group 4 | Control group 5 | Control group 6 |
| Iodine absorption value（mg/g） | 16.2 | 16.4 | 26.7 | 22.5 | 20.8 | 16.2 | 16.5 |
| Wearability improves ratio（%） | 36.3 | -2.6 | 39.9 | 39.7 | 40.3 | -1.9 | -1.4 |
As shown in Table 2, it is that 8.2% sulfuric acid soaks 5.3 hours by carbon black concentration, is washed repeatedly to neutrality with water, then use saturated carbon
Sour hydrogen sodium soaks 1.1 hours, is washed repeatedly to neutrality with water；It is best to reducing carbon black iodine absorption number effect, and arbitrarily cancel 8.2%
Sulfuric acid soaks 5.3 hours or soaked 1.1 hours with saturated sodium bicarbonate acts on equal unobvious to reducing carbon black iodine absorption number, will locate
Carbon black after reason is calcined 32 minutes at 485 DEG C, rapid to be sent into cold shock in frozen water, is pulled out, is dried, and is had to improving carbon black wearability
Remarkable effect, but arbitrarily reduction or increasing calcining temperature, then can not necessarily play and improve carbon black wearability effect, or even can drop
Low carbon black wearability.
Embodiment 3：A kind of production method of modified carbon black, specific processing step are as follows：
It is that 8.5% sulfuric acid soaks 5.5 hours by carbon black concentration, is washed repeatedly to neutrality with water, then soaked with saturated sodium bicarbonate
1.3 hours, washed repeatedly to neutrality with water；
Carbon black after processing is calcined 35 minutes at 490 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
It is HS22 carbon blacks as modification object to select kind, be divided at random experimental group, control group 1, control group 2,
Totally 7 groups of control group 3, control group 4, control group 5, control group 6；
Experimental group is modified processing according to the mode of embodiment 3；
The cancellation step on the basis of embodiment 3 of control group 1（2）Carbon black is modified；
The cancellation step on the basis of embodiment 3 of control group 2（1）Carbon black is modified；
Control group 3 is cancelled concentration on the basis of embodiment 3 and carbon black was modified in 5 hours for the immersion of 8% sulfuric acid；
The cancellation on the basis of embodiment 3 of control group 4 is soaked 1 hour with saturated sodium bicarbonate to be modified to carbon black；
The carbon black on the basis of embodiment 3 of control group 5 is calcined to be substituted for for 35 minutes at 490 DEG C calcines carbon black at 470 DEG C
Carbon black was modified in 35 minutes；
The carbon black on the basis of embodiment 3 of control group 6 is calcined to be substituted for for 35 minutes at 490 DEG C calcines carbon black at 520 DEG C
Carbon black was modified in 35 minutes；
Iodine absorption value and wear-resisting value after each group modification are detected, and calculates wearability and improves ratio, wearability improves ratio
Calculation formula is：（The wear-resisting value of modified wear-resisting value-before modified）/ wear-resisting value before modified, as a result see the table below 3：
| Group | Experimental group | Control group 1 | Control group 2 | Control group 3 | Control group 4 | Control group 5 | Control group 6 |
| Iodine absorption value（mg/g） | 15.0 | 15.1 | 23.4 | 16.5 | 17.0 | 15.5 | 15.3 |
| Wearability improves ratio（%） | 36.8 | -2.4 | 39.3 | 39.5 | 40.2 | -1.3 | -1.6 |
As shown in Table 3, it is that 8.5% sulfuric acid soaks 5.5 hours by carbon black concentration, is washed repeatedly to neutrality with water, then use saturated carbon
Sour hydrogen sodium soaks 1.3 hours, is washed repeatedly to neutrality with water；It is best to reducing carbon black iodine absorption number effect, and arbitrarily cancel 8.5%
Sulfuric acid soaks 5.5 hours or soaked 1.3 hours with saturated sodium bicarbonate acts on equal unobvious to reducing carbon black iodine absorption number, will locate
Carbon black after reason is calcined 35 minutes at 490 DEG C, rapid to be sent into cold shock in frozen water, is pulled out, is dried, and is had to improving carbon black wearability
Remarkable effect, but arbitrarily reduction or increasing calcining temperature, then can not necessarily play and improve carbon black wearability effect, or even can drop
Low carbon black wearability.
Embodiment 4：A kind of production method of modified carbon black, specific processing step are as follows：
It is that 8.8% sulfuric acid soaks 5.7 hours by carbon black concentration, is washed repeatedly to neutrality with water, then soaked with saturated sodium bicarbonate
1.4 hours, washed repeatedly to neutrality with water；
Carbon black after processing is calcined 38 minutes at 495 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
It is XT1004 carbon blacks as modification object to select kind, is divided into experimental group, control group 1, control group at random
2nd, totally 7 groups of control group 3, control group 4, control group 5, control group 6；
Experimental group is modified processing according to the mode of embodiment 4；
The cancellation step on the basis of embodiment 4 of control group 1（2）Carbon black is modified；
The cancellation step on the basis of embodiment 4 of control group 2（1）Carbon black is modified；
Control group 3 is cancelled concentration on the basis of embodiment 4 and carbon black was modified in 5 hours for the immersion of 8% sulfuric acid；
The cancellation on the basis of embodiment 4 of control group 4 is soaked 1 hour with saturated sodium bicarbonate to be modified to carbon black；
The carbon black on the basis of embodiment 4 of control group 5 is calcined to be substituted for for 38 minutes at 495 DEG C calcines carbon black at 470 DEG C
Carbon black was modified in 35 minutes；
The carbon black on the basis of embodiment 4 of control group 6 is calcined to be substituted for for 38 minutes at 495 DEG C calcines carbon black at 520 DEG C
Carbon black was modified in 35 minutes；
Iodine absorption value and wear-resisting value after each group modification are detected, and calculates wearability and improves ratio, wearability improves ratio
Calculation formula is：（The wear-resisting value of modified wear-resisting value-before modified）/ wear-resisting value before modified, as a result see the table below 4：
| Group | Experimental group | Control group 1 | Control group 2 | Control group 3 | Control group 4 | Control group 5 | Control group 6 |
| Iodine absorption value（mg/g） | 15.3 | 15.2 | 22.7 | 18.8 | 18.5 | 15.0 | 15.1 |
| Wearability improves ratio（%） | 36.5 | -2.1 | 39.0 | 39.4 | 40.5 | -1.2 | -1.5 |
As shown in Table 4, it is that 8.8% sulfuric acid soaks 5.7 hours by carbon black concentration, is washed repeatedly to neutrality with water, then use saturated carbon
Sour hydrogen sodium soaks 1.4 hours, is washed repeatedly to neutrality with water；It is best to reducing carbon black iodine absorption number effect, and arbitrarily cancel 8.8%
Sulfuric acid soaks 5.7 hours or soaked 1.4 hours with saturated sodium bicarbonate acts on equal unobvious to reducing carbon black iodine absorption number, will locate
Carbon black after reason is calcined 38 minutes at 495 DEG C, rapid to be sent into cold shock in frozen water, is pulled out, is dried, and is had to improving carbon black wearability
Remarkable effect, but arbitrarily reduction or increasing calcining temperature, then can not necessarily play and improve carbon black wearability effect, or even can drop
Low carbon black wearability.
Embodiment 5：A kind of production method of modified carbon black, specific processing step are as follows：
It is that 10% sulfuric acid soaks 6 hours by carbon black concentration, is washed repeatedly to neutrality with water, then 1.5 are soaked with saturated sodium bicarbonate
Hour, washed repeatedly to neutrality with water；
Carbon black after processing is calcined 40 minutes at 500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
Claims (5)
1. a kind of production method of modified carbon black, it is characterised in that specific processing step is as follows：
By carbon black with concentration be 8-10% sulfuric acid immersion 5-6 hours, washed repeatedly to neutrality with water, then soaked with saturated sodium bicarbonate
1-1.5 hours are steeped, are washed repeatedly to neutrality with water；
Carbon black after processing is calcined into 30-40 minutes at 480-500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain
To modified carbon black.
A kind of 2. production method of modified carbon black according to claim 1, it is characterised in that
It is that 8% sulfuric acid soaks 6 hours by carbon black concentration, is washed repeatedly to neutrality with water, then 1.5 are soaked with saturated sodium bicarbonate
Hour, washed repeatedly to neutrality with water.
A kind of 3. production method of modified carbon black according to claim 1, it is characterised in that
It is that 10% sulfuric acid soaks 5 hours by carbon black concentration, is washed repeatedly to neutrality with water, then it is small with saturated sodium bicarbonate immersion 1
When, washed repeatedly to neutrality with water.
A kind of 4. production method of modified carbon black according to claim 1, it is characterised in that
Carbon black after processing is calcined 40 minutes at 480 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
A kind of 5. production method of modified carbon black according to claim 1, it is characterised in that
Carbon black after processing is calcined 30 minutes at 500 DEG C, it is rapid to be sent into cold shock in frozen water, pull out, dry, obtain Modified Activated Carbon
It is black.
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Cited By (4)
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| CN110343341A (en) * | 2019-07-19 | 2019-10-18 | 四川宏亿复合材料工程技术有限公司 | A kind of ethylene propylene diene rubber and preparation method thereof |
| CN112976478A (en) * | 2021-02-02 | 2021-06-18 | 宁国市瑞普密封件有限公司 | Preparation method of automobile shock absorber bushing |
| CN113337143A (en) * | 2021-05-31 | 2021-09-03 | 安徽德瑞新材料科技有限公司 | Processing technology of special carbon black for high-pigment automobile finish |
| CN113429809A (en) * | 2021-05-31 | 2021-09-24 | 安徽德瑞新材料科技有限公司 | Processing technology of carbon black for ultrablue phase color matching |
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Application publication date: 20180126 |