CN106608628A - Method for preparing Chinese date pit activated carbon by zinc chloride activation - Google Patents

Method for preparing Chinese date pit activated carbon by zinc chloride activation Download PDF

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Publication number
CN106608628A
CN106608628A CN201611165952.4A CN201611165952A CN106608628A CN 106608628 A CN106608628 A CN 106608628A CN 201611165952 A CN201611165952 A CN 201611165952A CN 106608628 A CN106608628 A CN 106608628A
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CN
China
Prior art keywords
activated carbon
drying
zinc chloride
chinese date
semen jujubae
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Pending
Application number
CN201611165952.4A
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Chinese (zh)
Inventor
刘世军
唐志书
宋忠兴
高森
崔春利
刘红波
梁艳妮
张娱
许洪波
蔡兴航
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Shaanxi University of Chinese Medicine
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Shaanxi University of Chinese Medicine
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Priority to CN201611165952.4A priority Critical patent/CN106608628A/en
Publication of CN106608628A publication Critical patent/CN106608628A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/90Other properties not specified above

Abstract

The invention discloses a method for preparing Chinese date pit activated carbon by zinc chloride activation. The method comprises the following steps: putting Chinese date pits into a drying oven, drying at 105 DEG C, smashing after drying is finished, sieving by a No.7 sieve, dipping in five times of amounts of 50% zinc chloride solution prepared in advance for 24h, draining, and drying at 105 DEG C for standby application; preheating an electric cooker, putting the drained and dried Chinese date pit powder in a small tea china, sealing by another small tea china, inversely buckling by a stainless steel basin, completely sealing a gap by wet sand, calcining at a medium baking temperature for 25min, cooling to be at a room temperature, and opening to collect a sample; washing the sample with water to be neutral, levigating by a mortar after drying at 105 DEG C, and carrying out sealing storage to obtain the activated carbon. The activated carbon prepared with a calcined method has the advantages of simple and easy technology and stable finished product quality, a yield is 45.4%, an iodine sorption value is 891.69mg/g, and methylene blue decolourization capacity is 278.65ml/g.

Description

The method that zinc chloride activation prepares Semen Jujubae activated carbon
Technical field
The present invention relates to field of material preparation, and in particular to a kind of method that zinc chloride activation prepares Semen Jujubae activated carbon.
Background technology
Fructus Jujubae is sweet, warm, returns spleen, stomach, with invigorating the spleen and replenishing QI, effect of nourishing blood to tranquillize the mind.Can produce in large-scale production process The substantial amounts of Fructus Jujubae slag of life, Semen Jujubae., as garbage discarding, the waste of ample resources can be caused if by Semen Jujubae, can also be polluted Environment.Modern study shows in big Semen Jujubae rich in lignin and mineral, the great potential with exploitation wood activated charcoal.
China is the country of forest reserves shortage, and Fructus Jujubae is big in China's cultivated area, and distribution is wide, and yield is big.With original Material is that timber is raw material production activated carbon, and this has not only increased the contradiction of China's timber supply and demand, and destroys originally unstable Fixed ecological balance, in this sense, has very important significance to reasonable utilization of Semen Jujubae resource.Research shows, It is the good material for developing wood activated charcoal rich in lignin and mineral in big Semen Jujubae.The original of wood activated charcoal is prepared at present Material major part is agricultural product such as Semen Juglandiss shell, coconut husk, almond etc..Although and substantial amounts of Fructus Jujubae nucleocapsid is also by as being prepared into wood The excellent material of activated carbon, but have no the relevant report that wood activated charcoal is prepared into using the secretly method of forging.
The content of the invention
To solve the above problems, the invention provides a kind of method that zinc chloride activation prepares Semen Jujubae activated carbon, with the method for forging Prepare activated carbon process simple, end product properties are stable.
For achieving the above object, the technical scheme taken of the present invention is:
The method that zinc chloride activation prepares Semen Jujubae activated carbon, comprises the steps:
S1, big Semen Jujubae is put into baking oven, 105 DEG C of dryings after the completion of being dried, crushed No. seven sieves, were matched somebody with somebody in advance with 5 times of amounts The liquor zinci chloridi dipping 24h of 50% for making, drains, and 105 DEG C of drying are standby;
S2, first Electric stove preheated, then will be drained and dried big Semen Jujubae powder is put in little tea china, with another little porcelain Dish is closed, then uses Stainless steel basin back-off, with wet sand that gap closing is complete, opens moderate heat, and calcine 25min is cooled to room Temperature, opens, and collects sample;
S3, samples with water is rinsed to neutrality, after 105 DEG C of drying, ground with mortar, cross No. nine sieves, sealing preserve is Activated carbon.
The invention has the advantages that:
Prepare that activated carbon process is simple with the method for forging, end product properties are stable, and yield is 45.4%, and iodine sorption value is 891.69mg/g, Methylene blue adsorption is 278.65ml/g.
Description of the drawings
Fig. 1 is the relation of calcine time and activated carbon yield in the embodiment of the present invention.
Fig. 2 is the relation of calcine time and activated carbon-iodine adsorptive value in the embodiment of the present invention.
Fig. 3 is the relation of calcine time and activated carbon Methylene blue adsorption in the embodiment of the present invention.
Specific embodiment
In order that objects and advantages of the present invention become more apparent, the present invention is carried out further with reference to embodiments Describe in detail.It should be appreciated that specific embodiment described herein is not used to limit this only to explain the present invention It is bright.
In following examples, the material for being used is:
Big Semen Jujubae (laboratory self-control);95% ethanol (Anhui An Te food limited company product);Zinc chloride (Chongqing Mao Ye chemical reagent company limited);Iodine (Tianjin day man of great strength's chemical reagent company limited);Potassium iodide (Tianjin day man of great strengthization Learn reagent company limited);Sodium thiosulfate (Tianjin day man of great strength's chemical reagent company limited);Soluble starch (Chongqing cyclopentadienyl industry Chemical reagent company limited);Potassium dichromate (Chongqing Mao Ye chemical reagent company limited);Methylene blue (Chongqing cyclopentadienyl industry chemistry examination Agent company limited);Disodium hydrogen phosphate (Xi'an San Pu chemical reagent company limited);Potassium dihydrogen phosphate (Xi'an San Pu chemical reagent Company limited);Methylene blue test liquid (Xi'an San Pu chemical reagent company limited).
Embodiment
The preparation technology of the present embodiment activated → drained including big Semen Jujubae crushing → activator → and calcine method → washing → dry Dry → to pulverize and sieve → activated carbon;Specifically include following steps:
Big Semen Jujubae is put into into baking oven, 105 DEG C of dryings after the completion of being dried, were crushed No. seven sieves, and prepared in advance with 5 times of amounts 50% liquor zinci chloridi dipping 24h, drain.Then 105 DEG C of drying, standby.First Electric stove is preheated, then will be drained and be done Dry good sample, in being put into little tea china, is closed with another little tea china, then uses Stainless steel basin back-off, sub by gap with wet sand Closing is complete, opens moderate heat, starts timing, respectively the calcine time 15,20,25,30min, is cooled to room temperature.Open, collect sample Product, samples with water is rinsed to neutrality, after 105 DEG C of drying, is ground with mortar, crosses No. nine sieves, and sealing preserve is activated carbon.
According to the measure (GB/ of National Standard of the People's Republic of China's wood activated charcoal test method iodine sorption value T12496.8-1999), wood activated charcoal method of inspection Methylene blue adsorption (GB/T12496.2-90), to prepared work Property charcoal performance is measured.
Impact of the calcine time to activated carbon yield
When the calcine time 25min is extended to from 20min, the yield of activated carbon is reduced to 45.4% from 45.7%;With forging The prolongation of time processed, carburizing reagent carries out more abundant, and ablated surface carbon is continuously increased, and forms substantial amounts of micropore, causes The yield of activated carbon declines, but yield decline and it is whether apparent.As a result Fig. 1 is seen.
Impact of the calcine time to activated carbon-iodine adsorptive value
Iodine sorption value comes as seen from Figure 2 for representing absorbability of the activated carbon to liquid substance, what Semen Jujubae was produced The iodine sorption value of activated carbon increases with the growth of calcine time, and reaches peak value in 25min, such as the calcine time Extend, the degree of activation is gradually deepened, and the micropore and mesopore of formation also progressively increase, its pore structure is also just more and more flourishing, Meanwhile, with the prolongation of calcine time, calcine may be continued and cause the destruction of Microporous Structure of Active Carbon, and then make under iodine sorption value Drop.
Impact of the calcine time to activated carbon Methylene blue adsorption
Methylene blue adsorption is used to indicate that the foundation of activated carbon decolorizing ability.From the figure 3, it may be seen that methylene blue is de- Color power reaches peak value in 25min, and the decolorizing ability of this moment calcine activated carbon out is most strong, and then Methylene blue adsorption is opened Begin on a declining curve, it may be possible to which lasting high temperature calcine result in the microcellular structure of script to be occurred damaging, and causes methylene blue to decolourize The decline of power.
In the case where other conditions are constant, the calcine time directly decides the degree of activation.With prolonging for calcine time Long, yield, iodine sorption value, the Methylene blue adsorption of Semen Jujubae activated carbon are stepped up and then decline.So the calcine time is not Oversize, the long-time high temperature of energy, the microcellular structure structure that the suitable activated carbon that has been carbonized originally is caused on the contrary is damaged, and then The functional characteristic of activated carbon is affected, the decline of Properties of Activated Carbon is caused.In order to take into account activated carbon adsorption performance and yield, select most Good soak time is 25min.
In calcination process, because Semen Jujubae is heated carbonization, there are a large amount of gases and dense smoke to spray from pot seam, it should to use in time Wet sand is blocked, and is entered with anti-pollution environment and air, makes sample ashing.Time will cut off the electricity supply in time to after, place to room Temperature opens again button basin.If opening button basin too early, sample contact oxygen can be caused and resume combustion, and then increase experimental error
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (1)

1. the method that zinc chloride activation prepares Semen Jujubae activated carbon, it is characterised in that comprise the steps:
S1, big Semen Jujubae is put into baking oven, 105 DEG C of dryings after the completion of being dried, crushed No. seven sieves, is prepared in advance with 5 times of amounts 50% liquor zinci chloridi dipping 24h, drains, and 105 DEG C of drying are standby;
S2, first Electric stove preheated, then will be drained and dried big Semen Jujubae powder is put in little tea china, sealed with another little tea china Close, then use Stainless steel basin back-off, it is with wet sand that gap closing is complete, moderate heat is opened, calcine 25min is cooled to room temperature, beats Open, collect sample;
S3, samples with water is rinsed to neutrality, after 105 DEG C of drying, ground with mortar, cross No. nine sieves, sealing preserve is activity Charcoal.
CN201611165952.4A 2016-12-16 2016-12-16 Method for preparing Chinese date pit activated carbon by zinc chloride activation Pending CN106608628A (en)

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CN201611165952.4A CN106608628A (en) 2016-12-16 2016-12-16 Method for preparing Chinese date pit activated carbon by zinc chloride activation

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101966990A (en) * 2010-11-15 2011-02-09 西北农林科技大学 Method for preparing activated carbon from kernel of common macrocarpium fruit
CN102745685A (en) * 2012-07-18 2012-10-24 太仓市联林活性炭厂 Process of using dogwood kernel to prepare activated carbon
CN103303917A (en) * 2013-07-25 2013-09-18 程俊校 Activated carbon and preparation process thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101966990A (en) * 2010-11-15 2011-02-09 西北农林科技大学 Method for preparing activated carbon from kernel of common macrocarpium fruit
CN102745685A (en) * 2012-07-18 2012-10-24 太仓市联林活性炭厂 Process of using dogwood kernel to prepare activated carbon
CN103303917A (en) * 2013-07-25 2013-09-18 程俊校 Activated carbon and preparation process thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
湖北中医学院编: "《炮制学讲义》", 30 April 1974 *

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Application publication date: 20170503

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