CN105460932B - The method for purifying cocoanut active charcoal - Google Patents
The method for purifying cocoanut active charcoal Download PDFInfo
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Abstract
The present invention discloses a kind of method for purifying cocoanut active charcoal, and it includes：Rough cocoanut active charcoal is dried, recycles hydrogen peroxide and ethanol postincubation, recycles high-temperature vapor double rinse, last cool drying obtains cocoanut active charcoal of the present invention.The present invention utilizes the processing method of chemical bond physics, and obtained activated carbon is purer, and mesopore coverage rate is higher.The present invention, to Activated Carbon Pretreatment, is reprocessed to activated carbon using alcohol using hydrogen peroxide, recycles high-temperature vapor to post-process activated carbon, improve the degree of purity of activated carbon and the content of mesopore.The present invention penetrates into hydrogen peroxide inside activated carbon, recycles neutral spirits to absorb activated carbon internal moisture, improves the concentration of hydrogen peroxide, finally rinsed using high-temperature steam, hydrogen peroxide is fiercely decomposed into moisture and oxygen, so as to increase the middle hole number of activated carbon.
Description
Technical field
The present invention relates to activated carbon to purify field, it is more particularly related to a kind of side for purifying cocoanut active charcoal
Method.
Background technology
Cocoanut active charcoal is that cocoanut shell is raw material, is obtained by carbonization and purifying technique, cocoanut active charcoal has hole hair
Reach, absorption property is good, intensity is high, easy regeneration, economy and durability the advantages that, product is mainly used in taste removal, Drinking Water Filtration etc., is one
The emerging water-purifying material of kind.
The carbonization of cocoanut shell includes two methods of chemistry carbonization and physics carbonization, and cocoanut shell is exactly placed in by physics carbonizatin method
In retort, destructive distillation and anaerobic carbonization are carried out under the high temperature conditions.The cocoanut active charcoal obtained by physics carbonizatin method contains perhaps
More impurity, it is therefore desirable to carry out the purification processes in later stage.
The later purification processing method of activated carbon also includes two kinds of chemical method and Physical, and chemical method purification can reduce work
Ash and harmful substance in property charcoal, but the activity of activated carbon is greatly reduced, and new harmful substance is introduced, cause activity
The application field of charcoal is restricted.
Traditional physical purification method is directly to carry out boiling to activated carbon using vapor, and obtained activated carbon capillary compares
Prosperity, specific surface area is higher, but mesopore is not very flourishing, limits the application of activated carbon, therefore invention one kind can improve
The problem of method of purification of the activated coco nut charcoal of mesopore coverage rate is referred to as urgent need to resolve.
The content of the invention
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
Object of the present invention is to provide a kind of method for purifying cocoanut active charcoal, and it uses the processing of chemical bond physics
Method, obtained activated carbon is purer, and mesopore coverage rate is higher.
A further object of the invention is that Activated Carbon Pretreatment is located again using alcohol to activated carbon using hydrogen peroxide
Reason, recycle high-temperature vapor to post-process activated carbon, improve the degree of purity of activated carbon and the content of mesopore.
A further object of the invention is to penetrate into hydrogen peroxide inside activated carbon, recycles neutral spirits to absorb inside activated carbon
Moisture, the concentration of hydrogen peroxide is improved, is finally rinsed using high-temperature steam, hydrogen peroxide is fiercely decomposed into moisture and oxygen, from
And increase the middle hole number of activated carbon.
In order to realize according to object of the present invention and further advantage, there is provided a kind of side for purifying cocoanut active charcoal
Method, wherein, including：
Step 1: rough cocoanut active charcoal is dried to constant weight at 80-85 DEG C, then it is in the concentration of 1-10 times of volume
2-2.5h is soaked in 27-35% hydrogen peroxide, is filtrated to get product A；Cocoanut active charcoal drying to constant weight can be avoided into coconut husk
In the influence to hydrogen peroxide of moisture and other compositions, and dried cocoanut active charcoal can absorb and permeate more dioxygens
Water, after hydrogen peroxide enters activated carbon, the inside of activated carbon is rested on, hydrogen peroxide, can be to work during activated carbon is penetrated into
Property charcoal carry out slight oxidation, so as to which the aperture of expansion micropore by a small margin forms mesopore, increase the quantity of mesopore.Activated carbon
Micropore size typically in below 1nm, air molecule can be filtered, mesopore pore size can be used for pair typically in more than 1nm
Gas absorption, liquid filtering and Application in Chemical Engineering etc., therefore the quantity for increasing mesopore can expand or the application neck of activated carbon
Domain.
Step 2: at 0-3 DEG C, will be soaked in alcohol that the concentration of products obtained therefrom A and 1-10 times of volume is 95-100%
30-35min, it is filtrated to get product B；After hydrogen peroxide enters activated carbon inside, using high concentration or pure alcohol by water
Divide and sponge, the hydrogen peroxide inside activated carbon becomes dense hydrogen peroxide, so as to effectively to the micropore inside activated carbon
Carry out oxidation and expand aperture, avoid carrying out over oxidation to the micropore outside activated carbon.Hydrogen peroxide and alcohol are under 0-3 DEG C of state
It will not react, therefore the security of reaction can be ensured.
Step 3: at 10-15 DEG C, products obtained therefrom B is stood into 0.5-3h, ventilation keeps 4-8m3/ min, obtains product
C；After the complete moisture of alcohol absorption, activated carbon is taken out stood rapidly, rapidly waved the alcohol on activated carbon using big ventilation
Hair removes, and reduces the content of alcohol as far as possible, avoids the influence to next step, has obtained the internal activated carbon containing hydrogen peroxide.
Step 4: 30-40min is rinsed to the products C of gained using the 860-870 DEG C of high-temperature steam that pressure is 3-4mpa,
Obtain product D；Activation process is carried out to activated carbon using high-temperature steam, high-temperature steam drives activated carbon continuous in reaction tank
Rolling, and the impurity in activated carbon is cemented out；Meanwhile the hydrogen peroxide inside activated carbon is decomposed into rapidly oxygen at high temperature
Gas and water, oxygen can make activated carbon form more holes, the filtering hole number of the activated carbon increased, improve activated carbon
Strainability.
Step 5: be continuing with the 760-770 DEG C of high-temperature steam that pressure is 4-5mpa rinses 70- to the product D of gained
90min, obtain product E；It is continuing with high-temperature vapor to activate activated carbon, substitutional impurity, cleans hydrogen peroxide or wine
The residues such as essence, make the brighter of activated carbon, purity is higher, due to hydrogen peroxide be completely decomposed at high temperature oxygen and
Water, alcohol are also rinsed totally, therefore obtained activated carbon does not have other impurities or a harmful substance, and the field of application is wider
It is wealthy.
Above step does not set stirring rod to be stirred activated carbon as conventional method, avoids activated carbon and hard
The collision of thing, reduce charcoal loss rate.
Step 6: products obtained therefrom E is removed, rinsed using atmospheric steam, until temperature drops to 110-115 DEG C, obtained
To product F；Vapor flushing is continuing with, makes activated carbon slow cooling, avoids huge temperature change from causing Properties of Activated Carbon
Influence.
Step 7: by products obtained therefrom F at 110-115 DEG C dry 13-15h i.e. obtain it is of the present invention coconut activated
Charcoal.Packaging is sealed up for safekeeping after activated carbon is dried.
Preferably, in the method for described purification cocoanut active charcoal, the preparation method of rough coconut husk described in step 1
For：After cocoanut shell is carbonized, the particle that particle diameter is 0.6-4mm is ground into, produces the rough cocoanut active charcoal.In order to improve work
Property efficiency and effect, cocoanut active charcoal are ground into certain size, then carry out activation process.
Preferably, in the method for described purification cocoanut active charcoal, physics is carried out to the cocoanut shell using carbonization machine
Carbonization.The carbonization of cocoanut shell includes Physical carbonization and chemical method carbonization, selects Physical using carbonization machine to cocoanut shell here
Mechanical carbonization is carried out, avoids introducing chemical impurity.
Preferably, in the method for described purification cocoanut active charcoal, using waterproof ventilated membrane to being utilized by step 5 after
Vapor filtered, collect the hot water filtered out and recycled.A kind of existing high polymer material of waterproof ventilated membrane, use
By the moisture filter in vapor and current can be congealed into herein, and gas can then be drained by air film.
Preferably, in the method for described purification cocoanut active charcoal, washing condition is time 35min in step 4, temperature
865 DEG C of degree, pressure 3.5mpa.For temperature at 865 degrees Celsius, the activation rate highest of carbon, the time, 35min was optimal again, long meeting
Increase the loss on ignition of activated carbon, yield rate reduces.
Preferably, in the method for described purification cocoanut active charcoal, washing condition is time 80min in step 5, temperature
765 DEG C of degree, pressure 4.5mpa.For temperature at 765 degrees Celsius, the activation rate of carbon is higher, and the time, 80min was optimal again, the process
The displacement and cleaning of impurity are mainly carried out to activated carbon, therefore temperature needs are lower, the time is longer.
Preferably, in the method for described purification cocoanut active charcoal, the concentration of hydrogen peroxide is 30% in the step 1.
The concentration of hydrogen peroxide is optimal with 30%, it is too high if before hydrogen peroxide does not penetrate into activated carbon inside by the outside of activated carbon
Oxidative demage, micropore that is too low and being not enough to magnesium oxide/absorbent charcoal.
The present invention comprises at least following beneficial effect：First, the chemical method of abandoning tradition activated carbon of the present invention purification and
Pure physical method, chemical method and physical method are combined, and both the impurity in scavenging capacity charcoal and harmful substance, and can were enough
The content of activated carbon mesopore is improved, while new harmful substance and impurity will not be introduced, therefore than traditional physico-chemical process
It is more environmentally-friendly effective.
Secondly, method of the invention does not need stirring rod to be stirred activated carbon, reduces the collision of activated carbon, reduces
Charcoal loss rate, and the method for the present invention does not reduce the mechanical wear-resisting intensity of activated carbon, the surface of activated carbon is brighter.
Again, method of the invention is soaked first by hydrogen peroxide to activated carbon, hydrogen peroxide is entered in activated carbon
Portion, expand the aperture of activated carbon, then recycle alcohol in high concentration to absorb the moisture in activated carbon, hydrogen peroxide is persisted activated carbon
Inside, finally activated carbon is rinsed using high-temperature vapor, fast decoupled under hydrogen peroxide high temperature is formed water and oxygen, this
A little oxygen can increase the aperture of activated carbon and increase the quantity in charcoal absorption hole.Whole process does not introduce new impurity,
Hydrogen peroxide used and alcohol are all decomposed or evaporated, therefore very clean and effective.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Embodiment
With reference to example, the present invention is described in further detail, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
Example 1
First, the preparation of activated carbon
After cocoanut shell is carbonized using carbonization machine, the particle that particle diameter is 0.85mm is ground into, produces rough cocoanut active charcoal；
Rough cocoanut active charcoal is dried to constant weight at 80 DEG C, is then to soak in 27% hydrogen peroxide in the concentration of 2 times of volumes
2h, it is filtrated to get product A；At 0 DEG C, by the concentration of products obtained therefrom A and 2 times of volumes be 95% alcohol in soak 35min, mistake
Filter obtains product B；At 10 DEG C, products obtained therefrom B is stood into 0.5h, ventilation keeps 8m3/ min, obtains products C；Use pressure
40min is rinsed to the products C of gained for 3mpa 860 DEG C of high-temperature steams, obtains product D；It is continuing with 760 that pressure is 4mpa
DEG C high-temperature steam rinses 90min to the product D of gained, obtains product E；Products obtained therefrom E is removed, rushed using atmospheric steam
Wash, until temperature drops to 110 DEG C, obtain product F；By products obtained therefrom F at 110 DEG C dry 15h i.e. obtain it is of the present invention
Cocoanut active charcoal.
2nd, performance test
The yield (i.e. the weight ratio of gained activated carbon and crude active charcoal) of cocoanut active charcoal of the present invention is determined, according to
Method as defined in national standard GB/T 12496.10-1999 carries out methylene blue adsorption value to cocoanut active charcoal of the present invention
Measure, is measured according to method as defined in GB/T 12496.5-1999 to carbon tetrachloride adsorption rate (activity), as a result such as following table
1：
It was found from upper table 1, the yield of activated carbon of the invention is up to the yield of 72% remote ultra-traditional method, methylene blue suction
Assignments and carbon tetrachloride adsorption rate are up to state standards.
Example 2
First, the preparation of activated carbon
After cocoanut shell is carbonized using carbonization machine, the particle that particle diameter is 1.4mm is ground into, produces rough cocoanut active charcoal；
Rough cocoanut active charcoal is dried to constant weight at 82 DEG C, is then to soak 2h in 30% hydrogen peroxide in the concentration of 5 times of volumes,
It is filtrated to get product A；At 3 DEG C, by the concentration of products obtained therefrom A and 5 times of volumes be 99.9% alcohol in soak 31min, mistake
Filter obtains product B；At 15 DEG C, products obtained therefrom B is stood into 3h, ventilation keeps 4m3/ min, obtains products C；It is using pressure
4mpa 870 DEG C of high-temperature steams rinse 30min to the products C of gained, obtain product D；It is continuing with 760 DEG C that pressure is 5mpa
High-temperature steam rinses 90min to the product D of gained, obtains product E；Products obtained therefrom E is removed, rinsed using atmospheric steam,
Until temperature drops to 115 DEG C, product F is obtained；By products obtained therefrom F at 115 DEG C dry 13h i.e. obtain it is of the present invention
Cocoanut active charcoal.
2nd, performance test
The yield (i.e. the weight ratio of gained activated carbon and crude active charcoal) of cocoanut active charcoal of the present invention is determined, according to
Method as defined in national standard GB/T 12496.10-1999 carries out methylene blue adsorption value to cocoanut active charcoal of the present invention
Measure, is measured according to method as defined in GB/T 12496.5-1999 to carbon tetrachloride adsorption rate (activity), as a result such as following table
2：
It was found from upper table 2, the yield of activated carbon of the invention is up to the yield of 75% remote ultra-traditional method, methylene blue suction
Assignments and carbon tetrachloride adsorption rate are up to state standards.
Example 3
First, the preparation of activated carbon
After cocoanut shell is carbonized using carbonization machine, the particle that particle diameter is 2mm is ground into, produces rough cocoanut active charcoal；Will
Rough cocoanut active charcoal is dried to constant weight at 83 DEG C, is then to soak 2h, mistake in 30% hydrogen peroxide in the concentration of 7 times of volumes
Filter obtains product A；At 0 DEG C, by the concentration of products obtained therefrom A and 7 times of volumes to soak 33min in 97% alcohol, filter
To product B；At 10 DEG C, products obtained therefrom B is stood into 2.5h, ventilation keeps 6m3/ min, obtains products C；It is using pressure
3.5mpa 865 DEG C of high-temperature steams rinse 35min to the products C of gained, obtain product D；It is 3.5mpa's to be continuing with pressure
765 DEG C of high-temperature steams rinse 80min to the product D of gained, obtain product E；Products obtained therefrom E is removed, uses atmospheric steam
Rinse, until temperature drops to 110 DEG C, obtain product F；Products obtained therefrom F is dried into 14h at 110 DEG C and obtains institute of the present invention
The cocoanut active charcoal stated.
2nd, performance test
The yield (i.e. the weight ratio of gained activated carbon and crude active charcoal) of cocoanut active charcoal of the present invention is determined, according to
Method as defined in national standard GB/T 12496.10-1999 carries out methylene blue adsorption value to cocoanut active charcoal of the present invention
Measure, is measured according to method as defined in GB/T 12496.5-1999 to carbon tetrachloride adsorption rate (activity), as a result such as following table
3：
It was found from upper table 3, the yield of activated carbon of the invention is up to the yield of 73% remote ultra-traditional method, methylene blue suction
Assignments and carbon tetrachloride adsorption rate are up to state standards.
Example 4
First, the preparation of activated carbon
After cocoanut shell is carbonized using carbonization machine, the particle that particle diameter is 2.8mm is ground into, produces rough cocoanut active charcoal；
Rough cocoanut active charcoal is dried to constant weight at 85 DEG C, is then to soak in 31% hydrogen peroxide in the concentration of 8 times of volumes
2.2h, it is filtrated to get product A；At 1 DEG C, by the concentration of products obtained therefrom A and 8 times of volumes to soak 33min in 99% alcohol,
It is filtrated to get product B；At 13 DEG C, products obtained therefrom B is stood into 2h, ventilation keeps 5m3/ min, obtains products C；Use pressure
38min is rinsed to the products C of gained for 3mpa 868 DEG C of high-temperature steams, obtains product D；It is 4.5mpa's to be continuing with pressure
766 DEG C of high-temperature steams rinse 85min to the product D of gained, obtain product E；Products obtained therefrom E is removed, uses atmospheric steam
Rinse, until temperature drops to 115 DEG C, obtain product F；Products obtained therefrom F is dried into 13h at 115 DEG C and obtains institute of the present invention
The cocoanut active charcoal stated.
2nd, performance test
The yield (i.e. the weight ratio of gained activated carbon and crude active charcoal) of cocoanut active charcoal of the present invention is determined, according to
Method as defined in national standard GB/T 12496.10-1999 carries out methylene blue adsorption value to cocoanut active charcoal of the present invention
Measure, is measured according to method as defined in GB/T 12496.5-1999 to carbon tetrachloride adsorption rate (activity), as a result such as following table
4：
It was found from upper table 4, the yield of activated carbon of the invention is up to the yield of 78% remote ultra-traditional method, methylene blue
Adsorptive value and carbon tetrachloride adsorption rate are up to state standards.
Example 5
First, the preparation of activated carbon
After cocoanut shell is carbonized using carbonization machine, the particle that particle diameter is 4mm is ground into, produces rough cocoanut active charcoal；Will
Rough cocoanut active charcoal is dried to constant weight at 82 DEG C, is then to soak 2h, mistake in 33% hydrogen peroxide in the concentration of 8 times of volumes
Filter obtains product A；At 0 DEG C, by the concentration of products obtained therefrom A and 10 times of volumes to soak 30min in 99% alcohol, filter
To product B；At 13 DEG C, products obtained therefrom B is stood into 2h, ventilation keeps 5m3/ min, obtains products C；The use of pressure is 3mpa
870 DEG C of high-temperature steams 38min is rinsed to the products C of gained, obtain product D；It is continuing with 760 DEG C of height that pressure is 4.5mpa
Warm steam rinses 85min to the product D of gained, obtains product E；Products obtained therefrom E is removed, rinsed using atmospheric steam, directly
115 DEG C are dropped to temperature, obtains product F；Products obtained therefrom F is dried into 13h at 115 DEG C and obtains coconut husk of the present invention
Activated carbon.
2nd, performance test
The yield (i.e. the weight ratio of gained activated carbon and crude active charcoal) of cocoanut active charcoal of the present invention is determined, according to
Method as defined in national standard GB/T 12496.10-1999 carries out methylene blue adsorption value to cocoanut active charcoal of the present invention
Measure, is measured according to method as defined in GB/T 12496.5-1999 to carbon tetrachloride adsorption rate (activity), as a result such as following table
5：
It was found from upper table 5, the yield of activated carbon of the invention is up to 69% and exceedes the yield of conventional method, methylene blue suction
Assignments and carbon tetrachloride adsorption rate are up to state standards.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With.It can be applied to various suitable the field of the invention completely., can be easily for those skilled in the art
Realize other modification.Therefore it is of the invention and unlimited under the universal limited without departing substantially from claim and equivalency range
In specific details and shown here as the example with description.
Claims (7)
1. a kind of method for purifying cocoanut active charcoal, wherein, including：
It is then 27- in the concentration of 1-10 times of volume Step 1: rough cocoanut active charcoal is dried to constant weight at 80-85 DEG C
2-2.5h is soaked in 35% hydrogen peroxide, is filtrated to get product A；
Step 2: at 0-3 DEG C, 30- will be soaked in alcohol that the concentration of products obtained therefrom A and 1-10 times of volume is 95-100%
35min, it is filtrated to get product B；
Step 3: at 10-15 DEG C, products obtained therefrom B is stood into 0.5-3h, ventilation keeps 4-8m3/ min, obtains products C；
Step 4: rinsing 30-40min to the products C of gained using the 860-870 DEG C of high-temperature steam that pressure is 3-4mpa, obtain
Product D；
Step 5: be continuing with the 760-770 DEG C of high-temperature steam that pressure is 4-5mpa rinses 70-90min to the product D of gained,
Obtain product E；
Step 6: products obtained therefrom E is removed, rinsed using atmospheric steam, until temperature drops to 110-115 DEG C, produced
Product F；
Step 7: it is to obtain described cocoanut active charcoal that products obtained therefrom F is dried into 13-15h at 110-115 DEG C.
2. the method for purification cocoanut active charcoal as claimed in claim 1, wherein, the preparation side of rough coconut husk described in step 1
Method is：After cocoanut shell is carbonized, the particle that particle diameter is 0.6-4mm is ground into, produces the rough cocoanut active charcoal.
3. the method for purification cocoanut active charcoal as claimed in claim 2, wherein, thing is carried out to the cocoanut shell using carbonization machine
Reason carbonization.
4. the method for purification cocoanut active charcoal as claimed in claim 1, wherein, using waterproof ventilated membrane to being utilized by step 5
Vapor afterwards is filtered, and is collected the hot water filtered out and is recycled.
5. the method for purification cocoanut active charcoal as claimed in claim 1, wherein, washing condition is time 35min in step 4,
865 DEG C of temperature, pressure 3.5mpa.
6. the method for purification cocoanut active charcoal as claimed in claim 1, wherein, washing condition is time 80min in step 5,
765 DEG C of temperature, pressure 4.5mpa.
7. the method for purification cocoanut active charcoal as claimed in claim 1, wherein, the concentration of hydrogen peroxide is in the step 1
30%.
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| CN106672969A (en) * | 2016-12-22 | 2017-05-17 | 桂东县湘浙活性炭有限公司 | Active carbon rinsing method |
| CN106698383B (en) * | 2017-01-20 | 2018-10-16 | 中天储能科技有限公司 | A method of LiFePO 4 material is prepared using coir fibre |
| CN110467179A (en) * | 2018-05-09 | 2019-11-19 | 上海核工程研究设计院有限公司 | A method of active carbon is handled with nuclear facilities radioactive liquid waste chemical flocculation |
| CN109437197A (en) * | 2018-12-15 | 2019-03-08 | 东莞理工学院 | A kind of mesoporous prosperity method for preparation of active carbon |
| CN109894078A (en) * | 2019-03-13 | 2019-06-18 | 湖北第二师范学院 | A kind of cocoanut active charcoal adsorbent material and manufacture craft based on water process |
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| CN104973597A (en) * | 2015-06-26 | 2015-10-14 | 河北德谦生物科技有限公司 | Production method of active carbon |
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Effective date of registration: 20190513 Address after: 536000 No. 41 Macau Road, Beihai Industrial Park, Guangxi Zhuang Autonomous Region (Room 103, Office Building, Beihai Horong Activated Carbon Technology Co., Ltd.) Patentee after: Beihai star stone carbon material technology Co., Ltd. Address before: No. 41 Macau Road, Beihai City, Guangxi Zhuang Autonomous Region, 536000 Patentee before: Beihai Herong Active Carbon Technology Co., Ltd. |
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Denomination of invention: Purification of coconut shell activated carbon Effective date of registration: 20210304 Granted publication date: 20171110 Pledgee: Beihai Xinyuan Investment Development Co.,Ltd. Pledgor: BEIHAI SENCE CARBON MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2021980001461 |