CN105217629A - The preparation method of coffee grounds gac - Google Patents
The preparation method of coffee grounds gac Download PDFInfo
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- CN105217629A CN105217629A CN201510723929.1A CN201510723929A CN105217629A CN 105217629 A CN105217629 A CN 105217629A CN 201510723929 A CN201510723929 A CN 201510723929A CN 105217629 A CN105217629 A CN 105217629A
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Abstract
The invention discloses a kind of preparation method of coffee grounds gac, comprise pre-treatment, de-oiling, dipping, the steps such as activation and cleaning, first also carbonized by the grease carried out coffee grounds in vacuum pyrolysis de-oiling removing coffee grounds and obtain coffee grounds carbon precursor, phosphoric acid is used to soak ultrasonic under different impregnating ratio (mass ratio of phosphoric acid and coffee grounds carbon precursor) as activator again, activate under different vacuum condition after drying, consider activation final temperature, vacuum tightness, temperature rise rate, soak time, the activation conditions such as impregnating ratio are on the impact of coffee grounds Properties of Activated Carbon, prepared coffee grounds gac yield is high, and iodine sorption value and methylene blue adsorption value have all exceeded national gac primary standard (iodine sorption value 1000mg/g, methylene blue adsorption value 135mg/g), can be used for the absorption to toxic and harmfuls such as the formaldehyde in room after fitting up, it is the extraordinary material for air purification of absorption property, whole carbon technique processed avoids the blocking of coffee grounds grease to coffee grounds gac hole, simple possible, duty parameter is stablized, environmental protection is pollution-free.
Description
Technical field
The present invention relates to waste recovery and utilize technical field, particularly a kind of preparation method of coffee grounds gac.
Background technology
Coffee, as first of the large beverage in the world three, is the second largest trade product being only second to oil, in daily life and commerce and trade, all has very important status.According to the statistics made by the departments concerned, Eleventh Five-Year Plan latter stage, China's coffee total cultivated area will be developed to more than 600,000 mu.From the whole world, to 2014, the output of coffee is 731.59 ten thousand tons/year, but often produces 1kg soluble coffee and will produce 0.9kg coffee grounds, how becomes new problem in recent years to coffee grounds recycling.
Along with the development of human society, the increase of environmental consciousness, gac is widely used in the field such as Industrial cleaning facility, environmental pollution prevention and control, but the scarcity of resource causes people from raw materials because usually selecting gac such as activation difficulty or ease, raw material grade, price, supplys, raw material turns to coal, oil etc. by wood material before, arrive comparatively cheap straw, coconut husk, jujube shell, bagasse, spent pulping liquor etc. again, but be that raw material is prepared gac and but rarely had research with coffee grounds.
Coffee grounds gac can be used as the peculiar smell that material for air purification comes in absorbed air, at present, medicine activation method has the advantage that carbonizes simultaneously and activate and is widely adopted, but the method is not proved effective to coffee grounds, reason is that coffee grounds contains a large amount of greases, these greases can block the hole of coffee grounds gac thus the activation effect of reduction medicine, therefore, how to slough the grease of coffee grounds and prepare the key that high performance gac is current techniques.
Summary of the invention
Task of the present invention is to provide a kind of vacuum pyrolysis and sloughs the grease of coffee grounds and obtain coffee grounds carbon precursor, then activates coffee grounds carbon precursor with phosphoric acid and obtain the preparation method of coffee grounds gac to solve prior art Problems existing.
The present invention is achieved through the following technical solutions goal of the invention:
The invention provides a kind of preparation method of coffee grounds gac, comprise the following steps:
(1) pre-treatment, washes away ash content and the water-soluble substances on coffee grounds surface with distilled water, then clean coffee grounds is placed in baking oven dry.
(2) de-oiling, is placed in vacuum pyrolysis device by the coffee grounds after dried in step (1), arranges temperature rise rate and vacuum tightness, rise to after de-oiling final temperature until temperature, and constant temperature makes coffee grounds carbonize de-oiling fat and obtains coffee grounds carbon matrix precursor;
(3) flood, take coffee grounds carbon matrix precursor in step (2) and be placed in beaker, add activator coffee soaking slag carbon matrix precursor by certain impregnating ratio (impregnating ratio is the mass ratio of phosphoric acid and coffee grounds precursor), ultrasonic, then dry;
(4) activate, the raw material after dried in step (3) is put into vacuum pyrolysis device and activates;
(5) clean, by the distilled water of step (4) gained coffee grounds gac certain temperature, lotion is extremely neutral repeatedly, carries out drying, cooling after suction filtration, and fully grinding obtains coffee grounds gac after sieving.
In order to extract the grease in coffee grounds as early as possible out, avoid coffee oil generation vigorous reaction simultaneously and be unfavorable for the recycling of each component in coffee oil, in step (2), the type of heating of vacuum pyrolysis device is external heat, and vacuum tightness is 0.02 ~ 0.08MPa, and temperature rise rate is 5 ~ 20 DEG C/min.
Further, de-oiling final temperature is 350 ~ 550 DEG C, and the constant temperature de-oiling time is 20 ~ 60min, thus, avoid the excessive pyrolysis of the too high coffee grounds of pyrolysis temperature generate tar and decrease the yield of coffee grounds carbon precursor, ensure that enough constant temperature times make coffee grounds oil ingredient all evaporate simultaneously.
Preferably, in step (2), the vacuum tightness of vacuum pyrolysis is 0.08MPa, and temperature rise rate is 10 DEG C/min, and de-oiling final temperature is 500 DEG C, and constant temperature soak time is 60min.
Further, in described step (3), activator is the mixing solutions of phosphoric acid and distilled water, selects phosphoric acid to activate, can improve the yield of gac, and activation temperature is low, can recycles of reduced contamination.
Further, in step (3), impregnating ratio is 0.5 ~ 2.0, and dipping time is 0.5 ~ 2h, and preferably, in step (3), impregnating ratio is 2.0, and dipping time is 2h.
Further, in step (3), distilled water volume is 10 ~ 50mL, ultrasonic time is 20 ~ 60min, drying temperature is 100 ~ 120 DEG C, and time of drying is 8 ~ 16h, and after flooding fully and be ultrasonic, phosphoric acid activation agent can penetrate into the inside of coffee grounds carbon matrix precursor fully.
Further, in step (4), the type of heating of vacuum pyrolysis device is external heat, activation vacuum tightness is 0.02 ~ 0.08MPa, activation temperature rise rate is 5 ~ 20 DEG C/min, activation temperature is 400 ~ 600 DEG C, constant temperature soak time is 0.5h ~ 2h, after fully activating, ether in coffee grounds carbon precursor forms macromolecular structure or strong bond, and oxygen and hydrogen mainly discharge as water vapor, decrease the organic generation of tarry, improve the yield of gac, and gac internal void can well be protected, improve the absorption property of coffee grounds gac.
Preferably, in step (4), the type of heating of vacuum pyrolysis device is external heat, and vacuum tightness is 0.08MPa, and temperature rise rate is 10 DEG C/min, and pyrolysis final temperature is 500 DEG C, and constant temperature soak time is 60min.
Further, in step (5), the temperature of distilled water is 40 ~ 80 DEG C, and the pH of neutral detergent solution is 6.0 ~ 7.0, and drying temperature is 100 ~ 120 DEG C, and time of drying is 8 ~ 16h.
Further, in step (1), drying temperature is 50 ~ 120 DEG C, and time of drying is 12 ~ 48h.
Further, step (2) also comprises and connects condenser system and non-condensable gas absorption system, thus, can the coffee grounds pyrolysis oil that produces of Separation and Recovery de-oiling fat, maximally utilise coffee grounds.
The preparation method of coffee grounds gac provided by the invention has the following advantages:
(1) blocking of coffee grounds grease to coffee grounds gac hole is avoided by vacuum pyrolysis de-oiling, capture the difficult point of coffee grounds grease blocking coffee grounds gac hole, Separation and Recovery coffee grounds pyrolysis oil utilizes as oil fuel or industrial chemicals simultaneously, fully utilizes to greatest extent coffee grounds.
(2) adopt phosphoric acid as activator, substantially increase the yield of coffee grounds gac, all can reach more than 30%, and consider the activation conditions such as activation final temperature, vacuum tightness, temperature rise rate, soak time, impregnating ratio to the impact of coffee grounds Properties of Activated Carbon comprehensively;
(3) the coffee grounds active carbon finished products prepared by records iodine sorption value 1312mg/g, methylene blue adsorption value 370mg/g according to the People's Republic of China (PRC) GB/T12496.8-1999 and GB/T12496.10-1999, all exceed national gac primary standard (iodine sorption value 1000mg/g, methylene blue adsorption value 135mg/g), can be used for the absorption to toxic gases such as the formaldehyde in room after fitting up, is the extraordinary material for air purification of absorption property.
(4) carbon sufficient raw processed, cheap, whole carbon technique simple possible processed, duty parameter is stablized, and environmental protection is pollution-free.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation:
List the activation temperature of the some embodiments of the present invention, vacuum tightness, soak time, impregnating ratio and temperature rise rate in table 1, wherein embodiment 17 to embodiment 21 is comparative example.
First with distilled water, the coffee grounds taking from Dongguan City, Guangdong Province soluble coffee factory is cleaned, remove impurity (ash content and water-soluble substances), clean coffee grounds is placed in 50 DEG C of oven drying 48h, get again dried after coffee grounds put into quartz boat and be placed in tube type resistance furnace, then condenser system and non-condensable gas absorption system is connected, check system starts vacuum pump without after gas leak phenomenon, under the numerical value regulating pressure valve that pyrolysis vacuum tightness is maintained in Table 1, regulate the parameter of tube type resistance furnace, heat up by the temperature rise rate in table 1, after arriving de-oiling final temperature 450 DEG C, pyrolysis de-oiling is carried out under de-oiling final temperature, constant temperature de-oiling 60min, about 50 DEG C are cooled to open silica tube after de-oiling terminates, coffee grounds carbon precursor can be obtained, and be separated and reclaim the coffee grounds pyrolysis oil in low-grade fever condenser system,
Take 10g coffee grounds carbon precursor and be placed in 100mL small beaker, the activator be made up of phosphoric acid 20g and 50mL distilled water is added by the impregnating ratio in table 1, wherein impregnating ratio is the mass ratio of phosphoric acid and coffee grounds carbon precursor, 2h is flooded and ultrasonic 1h after abundant mixing, then 105 DEG C of oven drying 12h are placed in, the coffee grounds carbon precursor flooded after dried is put into quartz boat and is placed in tube type resistance furnace, by numerical value in table 1, vacuum tightness is set respectively, temperature rise rate, treat that temperature rises to activation final temperature, by the soak time in table 1, obtained coffee grounds gac is activated to coffee grounds carbon precursor,
Again with the distilled water of about 80 DEG C repeatedly lotion be 7.0 to washings pH value, put into 105 DEG C of oven drying 12h after suction filtration; Fully grind and cross 200 mesh sieves after cooling, obtaining active carbon finished products.
The coffee grounds gac obtained to all embodiments records iodine sorption value and methylene blue adsorption value according to the People's Republic of China (PRC) GB/T12496.8-1999 and GB/T12496.10-1999, and test result is in table 1.
Table 1
As can be seen from Table 1, the present invention considers to activate final temperature comprehensively, vacuum tightness, temperature rise rate, soak time, after the activation parameters such as impregnating ratio, and adjustment activation final temperature 400-600 DEG C, vacuum tightness 0.02 ~ 0.08MPa, temperature rise rate 5 ~ 20 DEG C/min, soak time 20 ~ 120min, after impregnating ratio 0.5 ~ 2.0, the iodine sorption value of coffee grounds gac and methylene blue adsorption value all comparatively comparative example (embodiment 17-21) improve greatly, well beyond the iodine sorption value 1100mg/g of national Specification, methylene blue adsorption value 135mg/g, wherein, the adsorption effect of embodiment 12 is best.
Above-described is only some embodiments of the present invention.It should be understood that the content that those skilled in the art can announce according to the present invention carries out replacing and improving, but all replacements and improvement all do not depart from design of the present invention, these are replaced and improve the protection domain all belonging to appended claims of the present invention.
Claims (10)
1. a preparation method for coffee grounds gac, is characterized in that: the preparation method of described coffee grounds gac comprises the following steps:
(1) pre-treatment, washes away ash content and the water-soluble substances on coffee grounds surface with distilled water, then clean coffee grounds is placed in baking oven dry;
(2) de-oiling, is placed in vacuum pyrolysis device by the coffee grounds after dried in step (1), arranges temperature rise rate and vacuum tightness, rise to after de-oiling final temperature until temperature, and constant temperature makes coffee grounds carbonize de-oiling fat and obtains coffee grounds carbon matrix precursor;
(3) flood, take coffee grounds carbon matrix precursor in step (2) and be placed in beaker, add activator coffee soaking slag carbon matrix precursor by under certain impregnating ratio (mass ratio of activator solute and coffee grounds precursor), ultrasonic, then dry;
(4) activate, the raw material after dried in step (3) is put into vacuum pyrolysis device, temperature rise rate and vacuum tightness are set, rise to after activation final temperature until temperature, constant temperature activation is carried out to coffee grounds carbon matrix precursor;
(5) clean, by the distilled water of step (4) gained coffee grounds gac certain temperature, lotion is extremely neutral repeatedly, carries out drying, cooling after suction filtration, and fully grinding obtains coffee grounds gac after sieving.
2. the preparation method of coffee grounds gac according to claim 1, is characterized in that: in described step (2), the type of heating of vacuum pyrolysis device is external heat, and vacuum tightness is 0.02 ~ 0.08MPa, and temperature rise rate is 5 ~ 20 DEG C/min.
3. the preparation method of coffee grounds gac according to claim 2, is characterized in that: in described step (2), de-oiling final temperature is 350 ~ 550 DEG C, and the constant temperature de-oiling time is 20 ~ 60min.
4. the preparation method of coffee grounds gac according to claim 3, is characterized in that: in described step (3), activator is the mixing solutions of phosphoric acid and distilled water.
5. the preparation method of coffee grounds gac according to claim 4, is characterized in that: in described step (3), impregnating ratio is 0.5 ~ 2.0, and dipping time is 0.5 ~ 2h.
6. the preparation method of coffee grounds gac according to claim 5, is characterized in that: in described step (3), and distilled water volume is 10 ~ 50mL, and ultrasonic time is 20 ~ 60min, and drying temperature is 100 ~ 120 DEG C, and time of drying is 8 ~ 16h.
7. the preparation method of coffee grounds gac according to claim 6, it is characterized in that: in described step (4), the type of heating of vacuum pyrolysis device is external heat, vacuum tightness is 0.02 ~ 0.08MPa, temperature rise rate is 5 ~ 20 DEG C/min, activation temperature is 400 ~ 600 DEG C, and constant temperature soak time is 0.5h ~ 2h.
8. the preparation method of coffee grounds gac according to claim 7, is characterized in that: in described step (5), the temperature of distilled water is 40 ~ 80 DEG C, and the pH of neutral detergent solution is 6.0 ~ 7.0, and drying temperature is 100 ~ 120 DEG C, and time of drying is 8 ~ 16h.
9. the preparation method of coffee grounds gac according to claim 8, is characterized in that: in described step (1), drying temperature is 50 ~ 120 DEG C, and time of drying is 12 ~ 48h.
10. the preparation method of coffee grounds gac according to claim 9, is characterized in that: also comprise in described step (2) and connect condenser system and non-condensable gas absorption system.
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| CN107892300A (en) * | 2017-11-15 | 2018-04-10 | 广东环境保护工程职业学院 | A kind of coffee grounds valuable component separation and recovery method and application |
| CN108208277A (en) * | 2017-12-21 | 2018-06-29 | 苏州市佳禾食品工业有限公司 | A kind of method that coffee-extract is extracted from coffee grounds |
| CN108355620A (en) * | 2018-03-16 | 2018-08-03 | 唐山学院 | A kind of preparation of novel coffee slag matrix adsorbent and its remove chromium in water removal（VI）Application |
| CN108619851A (en) * | 2018-05-07 | 2018-10-09 | 中国农业大学 | A kind of preparation method to dehumidify except the coffee grounds packet with fresh air of formaldehyde |
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| CN110143592A (en) * | 2019-07-05 | 2019-08-20 | 咖法科技(上海)有限公司 | A kind of preparation method of coffee grounds active carbon |
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| CN112707396A (en) * | 2020-08-07 | 2021-04-27 | 王雪颖 | Phosphoric acid modified coffee grounds activated carbon and preparation method thereof |
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