CN106497151B - A kind of preparation method of polymolecularity carbon black - Google Patents
A kind of preparation method of polymolecularity carbon black Download PDFInfo
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- CN106497151B CN106497151B CN201610945520.9A CN201610945520A CN106497151B CN 106497151 B CN106497151 B CN 106497151B CN 201610945520 A CN201610945520 A CN 201610945520A CN 106497151 B CN106497151 B CN 106497151B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
Abstract
The present invention relates to a kind of preparation methods of polymolecularity carbon black, belong to polymolecularity black carbon technology field.The present invention generates carbon black by rapeseed oil imperfect combustion and is deposited on glass infuser inner wall, it scrapes spare, fermentation liquid is obtained with the biomass mixed fermentation rich in amino acid again, it is modified to carbon blacksurface under the methane liquid collective effect rich in microorganism using fermentation liquid, up to polymolecularity carbon black after spray drying.The present invention utilizes the fermentation liquid rich in amino acid modified to carbon blacksurface, increase the hydrophilic amino group and carboxyl quantity of carbon blacksurface under the action of microorganism, improve the hydrophily of carbon black, the carboxylic group in amino acid can form stable solvated layer in water simultaneously, agglomeration is avoided, makes carbon black that there is splendid water dispersible, it is poor with wettability to solve conventional carbon black, it is easy to reunite in water to be difficult to the problem of dispersing, have broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of polymolecularity carbon black, belong to carbon black preparation technical field.
Background technique
Carbon black is a kind of important chemical raw material, with excellent reinforcing, coloring, light resistance, antistatic property and
Ultraviolet-resistent property, and it is abundance, cheap, it has been widely used in rubber, plastics, ink, coating, dry cell and chemical fibre etc.
Many industries.Carbon black is the product of hydrocarbons imperfect combustion or cracking, can be divided into oven process, channel process and hot tearing by production method
Method.Wherein channel black is banned by many countries because yield is very low, environmental pollution is serious, and furnace black, especially oil oven
Method carbon black because yield is high, product quality is easy to control, it is low in the pollution of the environment due to become main kind of carbon black at present.
The main ingredient of carbon black is carbon, so that carbon black is in nonpolarity, it is poor with polar wettability, it is difficult in water point
It dissipates.Currently, in order to improve the self-dispersing and stability of carbon black in water, main preparation methods have oxidation modification, graft modification,
Dispersing agent directly disperses and polymer encapsulation, its essence is introducing or adsorbing hydrophilic radical in hydrophobic carbon blacksurface, makes
There is enough electrostatic repulsions and/or space resistance to prevent from assembling, to obtain stable aqueous carbon black dispersion between carbon black particle
Liquid.It is now recognized that the hydrophily of carbon black is mainly related with the acid functional mass contg of carbon blacksurface, and due to the dissociation of carboxyl
Constant is less than hydroxyl, and therefore, carboxyl disperses to play a major role in water to carbon black, they are capable of forming stable solvent in water
Change layer, while the cation in adsorption solvent forms double electrical layers, the repulsive force of generation can hinder the collision between carbon black pellet
Cohesion.
So far, have many research workers both at home and abroad and engage in carbon black Quality Research, such as coming to the surface for carbon black
Learn activity, form and microstructure and the surface nature of carbon black etc. to various surfactants and polymer carbon blacksurface suction
Attached, dispersion and its system performance have also made more research, but are not fully solved carbon black agglomeration traits again in water-based system yet.
Summary of the invention
The present invention solves the technical problem of: it is poor for current conventional carbon black and wettability, easy in water
It is poly- to be difficult to disperse, and common carbon black modified method cannot be fully solved carbon black in water-based system agglomeration traits again it is scarce
It falls into.The present invention generates carbon black by rapeseed oil imperfect combustion and is deposited on glass infuser inner wall, and scraping is spare, then with rich in amino
The biomass mixed fermentation of acid obtains fermentation liquid, using fermentation liquid to carbon black table under the methane liquid collective effect rich in microorganism
Face is modified, up to polymolecularity carbon black after spray drying.The present invention utilizes the fermentation liquid rich in amino acid modified to carbon blacksurface,
The hydrophilic amino group and carboxyl quantity for increasing carbon blacksurface under the action of microorganism, improve the hydrophily of carbon black, together
When amino acid in carboxylic group can form stable solvated layer in water, while adsorbing the cation in water and forming double electricity
Layer structure, the repulsive force of generation can hinder the collision between carbon black pellet to agglomerate, avoid agglomeration, and carbon black is made to have splendid water
Dispersibility, solves that conventional carbon black is poor with wettability, is easy the carbon black modified method for being difficult to disperse, and common of reuniting in water
It cannot be fully solved the problem of carbon black is reunited again in water-based system again, have broad application prospects.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) it measures 500~600mL rapeseed oil to be fitted into vial, then is added a long 10~15cm's into rapeseed oil
Cotton thread obtains self-control oil lamp as wick, puts and covers glass with the cylindric glass infuser of a 8~10cm of diameter after fuel-burning lamp
Bottle scrapes glass infuser inner wall silica aerogel layer with scraper, is put into until the rapeseed oil completely burnout in vial, glass infuser is taken out
It is put into baking oven dry 30~40min at 105~110 DEG C after 20~30min of mortar grinder, obtains hydrocarbon black powder, it is spare；
(2) it weighs 100~200g and climbs rock loach, 50~60g squid palpus out, 120~130g soya bean and 200~300g lotus root piece and be put into
20~30min is crushed in tissue pulverizer and obtains mixture, and mixture is fitted into ceramic pot, the matter such as mixture are added into tank
The deionized water of amount, sealed fermenter after mixing evenly, spontaneous fermentation 20~30 days；
(3) to it is above-mentioned after fermentation, take out fermentation material filtering removal filter residue, filtrate is obtained, by filtrate horizontal centrifugal
Machine is with 2000~3000r/min, 10~15min of revolving speed centrifugal treating, isolated supernatant, then supernatant is put into rotation and is steamed
It sends out in instrument, the 1/3 of concentrated by rotary evaporation to its original volume, obtains kilnitamin concentrate；
(4) with ultrasound point after above-mentioned kilnitamin concentrate and spare hydrocarbon black powder being mixed for 5:1 in mass ratio
Instrument is dissipated with 200~300W, 30~40min of power dispersion, obtains dispersion liquid, measures the methane liquid of the quality such as hydrocarbon black powder, centrifugation 10~
Methane liquid is clarified on the isolated upper layer 15min, then 9 will be fermented at 30~40 DEG C after clarification methane liquid and dispersion liquid mix~
12 days；
(5) to which after fermentation, fermentation material is put into vacuum concentration pot, pressure inside the tank is reduced to 900~1000Pa, is subtracted
Concentrate is obtained after 2~3h of pressure concentration, then will be packed after concentrate spray dryer drying up to polymolecularity carbon black.
The present invention utilizes the fermentation liquid rich in amino acid modified to carbon blacksurface, increases carbon black table under the action of microorganism
The hydrophilic amino group and carboxyl quantity in face, improve the hydrophily of carbon black, while the carboxylic group in amino acid can be
Stable solvated layer is formed in water, while adsorbing the cation in water and forming double electrical layers, and the repulsive force of generation can hinder
Collision cohesion between carbon black pellet, avoids agglomeration, carbon black is made to have splendid water dispersible.
The beneficial effects of the present invention are:
(1) there is excellent water dispersible using the carbon black of method provided by the invention production, preparation process is simple, operation
Property is strong, can promote and apply rapidly；
(2) polymolecularity carbon black produced by the present invention has good water dispersible and stability, and 5 are stood in normal-temperature water
~8 days, no precipitating and agglomeration generated.
Specific embodiment
It measures 500~600mL rapeseed oil to be fitted into vial, then the cotton thread of a long 10~15cm is added into rapeseed oil
As wick, self-control oil lamp is obtained, puts and covers vial with the cylindric glass infuser of a 8~10cm of diameter after fuel-burning lamp, directly
Rapeseed oil completely burnout into vial, glass infuser is taken out, and is scraped glass infuser inner wall silica aerogel layer with scraper, is put into mortar and grinds
It is put into baking oven dry 30~40min at 105~110 DEG C after 20~30min of mill, obtains hydrocarbon black powder, weighs 100~200g and climb
Rock loach, 50~60g squid palpus out, 120~130g soya bean and 200~300g lotus root piece are put into 20~30min of crushing in tissue pulverizer
Mixture is obtained, mixture is fitted into ceramic pot, the deionized water of the quality such as mixture is added into tank, it is close after mixing evenly
Seal fermentation tank, spontaneous fermentation 20~30 days；Fermentation material filtering removal filter residue is taken out, filtrate is obtained after fermentation to above-mentioned, it will
Filtrate with horizontal centrifuge with 2000~3000r/min, 10~15min of revolving speed centrifugal treating, isolated supernatant, then will be upper
Clear liquid is put into Rotary Evaporators, and the 1/3 of concentrated by rotary evaporation to its original volume, obtain kilnitamin concentrate；It is in mass ratio
5:1 is divided after mixing above-mentioned kilnitamin concentrate and spare hydrocarbon black powder with ultrasonic disperse instrument with 200~300W power
30~40min is dissipated, dispersion liquid is obtained, measures the methane liquid of the quality such as hydrocarbon black powder, the isolated upper layer clarification of 10~15min of centrifugation
Methane liquid, then by after clarification methane liquid and dispersion liquid mixing, ferment 9~12 days at 30~40 DEG C；To after fermentation, send out
Ferment object is put into vacuum concentration pot, is reduced pressure inside the tank and is obtained concentrate after 2~3h is concentrated under reduced pressure to 900~1000Pa, then will
It packs after concentrate spray dryer drying up to polymolecularity carbon black.
Example 1
500mL rapeseed oil is measured to be fitted into vial, then into rapeseed oil one long 10cm of addition cotton thread as wick,
Self-control oil lamp is obtained, with the cylindric glass infuser of a diameter 8cm covers vial after putting fuel-burning lamp, the dish in vial
Seed oil completely burnout, glass infuser is taken out, and is scraped glass infuser inner wall silica aerogel layer with scraper, is put into after being put into mortar grinder 20min
Baking oven dry 30min at 105 DEG C, obtains hydrocarbon black powder, weighs 100g and climb rock loach, 50g squid palpus out, 120g soya bean and 200g lotus root
Piece is put into crushing 20min in tissue pulverizer and obtains mixture, and mixture is fitted into ceramic pot, mixture etc. is added into tank
The deionized water of quality, sealed fermenter after mixing evenly, spontaneous fermentation 20 days；To it is above-mentioned after fermentation, take out fermentation material
Filtering removal filter residue, obtains filtrate, isolated by filtrate with horizontal centrifuge with 2000r/min revolving speed centrifugal treating 10min
Supernatant, then supernatant is put into Rotary Evaporators, the 1/3 of concentrated by rotary evaporation to its original volume, obtain kilnitamin concentration
Liquid；In mass ratio for 5:1 will above-mentioned kilnitamin concentrate and spare hydrocarbon black powder mix after with ultrasonic disperse instrument with
200W power dispersion 30min obtains dispersion liquid, measures the methane liquid of the quality such as hydrocarbon black powder, and the centrifugation isolated upper layer 10min is clear
Clear methane liquid, then by after clarification methane liquid and dispersion liquid mixing, ferment 9 days at 30 DEG C；To which after fermentation, fermentation material is put
Enter in vacuum concentration pot, reduces pressure inside the tank and obtain concentrate after 2h is concentrated under reduced pressure to 900Pa, then concentrate is done with spraying
It packs after dry device is dry up to polymolecularity carbon black.
There is an excellent dispersibility using the carbon black that the method disclosed in the present produces, simple production process, strong operability,
It is poor with wettability to solve conventional carbon black, being easy to reunite in water is difficult to the problem of dispersing, by carbon black produced by the present invention point
It is dispersed in normal-temperature water, stands 5 days, no precipitating and agglomeration generate, and have broad application prospects.
Example 2
600mL rapeseed oil is measured to be fitted into vial, then into rapeseed oil one long 15cm of addition cotton thread as wick,
Self-control oil lamp is obtained, with the cylindric glass infuser of a diameter 10cm covers vial after putting fuel-burning lamp, up in vial
Rapeseed oil completely burnout, glass infuser is taken out, and is scraped glass infuser inner wall silica aerogel layer with scraper, is put after being put into mortar grinder 30min
Enter baking oven dry 40min at 110 DEG C, obtains hydrocarbon black powder, weigh 200g and climb rock loach, 60g squid palpus out, 130g soya bean and 300g
Lotus root piece is put into crushing 30min in tissue pulverizer and obtains mixture, and mixture is fitted into ceramic pot, mixture is added into tank
Etc. quality deionized water, sealed fermenter after mixing evenly, spontaneous fermentation 30 days；To it is above-mentioned after fermentation, take out fermentation
Object filtering removal filter residue, obtains filtrate, filtrate is separated with horizontal centrifuge with 3000r/min revolving speed centrifugal treating 15min
It is put into Rotary Evaporators to supernatant, then by supernatant, the 1/3 of concentrated by rotary evaporation to its original volume, it is dense to obtain kilnitamin
Contracting liquid；In mass ratio for 5:1 will above-mentioned kilnitamin concentrate and spare hydrocarbon black powder mix after with ultrasonic disperse instrument with
300W power dispersion 40min obtains dispersion liquid, measures the methane liquid of the quality such as hydrocarbon black powder, and the centrifugation isolated upper layer 15min is clear
Clear methane liquid, then by after clarification methane liquid and dispersion liquid mixing, ferment 12 days at 40 DEG C；To after fermentation, by fermentation material
It is put into vacuum concentration pot, reduces pressure inside the tank and obtain concentrate after 3h is concentrated under reduced pressure to 1000Pa, then by concentrate with by spraying
It packs after drier is dry up to polymolecularity carbon black.
There is an excellent dispersibility using the carbon black that the method disclosed in the present produces, simple production process, strong operability,
It is poor with wettability to solve conventional carbon black, being easy to reunite in water is difficult to the problem of dispersing, by carbon black produced by the present invention point
It is dispersed in normal-temperature water, stands 7 days, no precipitating and agglomeration generate, and have broad application prospects.
Example 3
550mL rapeseed oil is measured to be fitted into vial, then into rapeseed oil one long 13cm of addition cotton thread as wick,
Self-control oil lamp is obtained, with the cylindric glass infuser of a diameter 9cm covers vial after putting fuel-burning lamp, the dish in vial
Seed oil completely burnout, glass infuser is taken out, and is scraped glass infuser inner wall silica aerogel layer with scraper, is put into after being put into mortar grinder 25min
Baking oven dry 35min at 108 DEG C, obtains hydrocarbon black powder, weighs 150g and climb rock loach, 55g squid palpus out, 125g soya bean and 250g lotus root
Piece is put into crushing 25min in tissue pulverizer and obtains mixture, and mixture is fitted into ceramic pot, mixture etc. is added into tank
The deionized water of quality, sealed fermenter after mixing evenly, spontaneous fermentation 25 days；To it is above-mentioned after fermentation, take out fermentation material
Filtering removal filter residue, obtains filtrate, isolated by filtrate with horizontal centrifuge with 2500r/min revolving speed centrifugal treating 13min
Supernatant, then supernatant is put into Rotary Evaporators, the 1/3 of concentrated by rotary evaporation to its original volume, obtain kilnitamin concentration
Liquid；In mass ratio for 5:1 will above-mentioned kilnitamin concentrate and spare hydrocarbon black powder mix after with ultrasonic disperse instrument with
250W power dispersion 35min obtains dispersion liquid, measures the methane liquid of the quality such as hydrocarbon black powder, and the centrifugation isolated upper layer 13min is clear
Clear methane liquid, then by after clarification methane liquid and dispersion liquid mixing, ferment 11 days at 35 DEG C；To after fermentation, by fermentation material
It is put into vacuum concentration pot, reduces pressure inside the tank and obtain concentrate after 3h is concentrated under reduced pressure to 950Pa, then by concentrate with by spraying
It packs after drier is dry up to polymolecularity carbon black.
There is an excellent dispersibility using the carbon black that the method disclosed in the present produces, simple production process, strong operability,
It is poor with wettability to solve conventional carbon black, being easy to reunite in water is difficult to the problem of dispersing, by carbon black produced by the present invention point
It is dispersed in normal-temperature water, stands 8 days, no precipitating and agglomeration generate, and have broad application prospects.
Claims (1)
1. a kind of preparation method of polymolecularity carbon black, it is characterised in that specific preparation step are as follows:
(1) it measures 500~600mL rapeseed oil to be fitted into vial, then the cotton thread of a long 10~15cm is added into rapeseed oil
As wick, self-control oil lamp is obtained, puts and covers vial with the cylindric glass infuser of a 8~10cm of diameter after fuel-burning lamp, directly
Rapeseed oil completely burnout into vial, glass infuser is taken out, and is scraped glass infuser inner wall silica aerogel layer with scraper, is put into mortar and grinds
It is transferred to baking oven after 20~30min of mill, dry 30~40min, obtains hydrocarbon black powder at 105~110 DEG C, spare；
(2) it weighs 100~200g and climbs rock loach, 50~60g squid palpus out, 120~130g soya bean and 200~300g lotus root piece and be put into tissue
20~30min is crushed in pulverizer and obtains mixture, and mixture is fitted into ceramic pot, the quality such as mixture are added into tank
Deionized water, sealed fermenter after mixing evenly, spontaneous fermentation 20~30 days；
(3) to it is above-mentioned after fermentation, take out fermentation material filtering removal filter residue, obtain filtrate, by filtrate with horizontal centrifuge with
2000~3000r/min, 10~15min of revolving speed centrifugal treating, isolated supernatant, then supernatant is put into Rotary Evaporators
In, the 1/3 of concentrated by rotary evaporation to its original volume, obtain kilnitamin concentrate；
(4) after in mass ratio above-mentioned kilnitamin concentrate and spare hydrocarbon black powder being mixed for 5:1 use ultrasonic disperse instrument
With 200~300W, 30~40min of power dispersion, dispersion liquid is obtained, measures the methane liquid of the quality such as hydrocarbon black powder, centrifugation 10~
Methane liquid is clarified on the isolated upper layer 15min, then 9 will be fermented at 30~40 DEG C after clarification methane liquid and dispersion liquid mix~
12 days；
(5) to which after fermentation, fermentation material is put into vacuum concentration pot, pressure inside the tank is reduced to 900~1000Pa, is depressurized dense
Concentrate is obtained after 2~3h of contracting, then will be packed after concentrate spray dryer drying up to polymolecularity carbon black.
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| CN107032882A (en) * | 2017-04-21 | 2017-08-11 | 董晓 | A kind of preparation method that type tobacco seedling medium can be recycled |
| CN110116999A (en) * | 2019-06-05 | 2019-08-13 | 张家港宝诚电子有限公司 | A kind of apparatus and method using paraffin preparation high-purity carbon |
| CN113248945A (en) * | 2021-05-20 | 2021-08-13 | 杭州君一新材料科技有限公司 | Treatment process of easy-to-disperse special carbon black |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101547858A (en) * | 2006-10-18 | 2009-09-30 | 新加坡科技研究局 | Method of functionalizing a carbon material |
| CN104628443A (en) * | 2015-01-27 | 2015-05-20 | 上海温兴生物工程有限公司 | Earthworm amino acid liquid organic fertilizer and production method thereof |
| CN105176811A (en) * | 2015-07-31 | 2015-12-23 | 华中农业大学 | System and method for utilizing biogas slurry and straw hydrolysate to prepare amino acid and separate CO2 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101547858A (en) * | 2006-10-18 | 2009-09-30 | 新加坡科技研究局 | Method of functionalizing a carbon material |
| CN104628443A (en) * | 2015-01-27 | 2015-05-20 | 上海温兴生物工程有限公司 | Earthworm amino acid liquid organic fertilizer and production method thereof |
| CN105176811A (en) * | 2015-07-31 | 2015-12-23 | 华中农业大学 | System and method for utilizing biogas slurry and straw hydrolysate to prepare amino acid and separate CO2 |
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