CN102942173B - Electric conduction dust-free health care carbon granule - Google Patents

Electric conduction dust-free health care carbon granule Download PDF

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Publication number
CN102942173B
CN102942173B CN201210481154.8A CN201210481154A CN102942173B CN 102942173 B CN102942173 B CN 102942173B CN 201210481154 A CN201210481154 A CN 201210481154A CN 102942173 B CN102942173 B CN 102942173B
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microwave
treatment
carbon granule
speed
temperature
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CN102942173A (en
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丁建中
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Yantai Power Intellectual Property Service Co.,Ltd.
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Zhejiang Builds And Hits Bamboo Scientific And Technological Co Ltd
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Abstract

The invention relates to the field of macromolecules, in particular to an electric conduction dust-free health care carbon granule. The granule is prepared through the following steps: pre-processing raw materials: placing plant raw materials into a microwave vacuum tank, vacuumizing, and conducting microwave processing; drying, pre-carbonizing, carbonizing, calcining and cooling sequentially, controlling burning to raise the temperature to 700-750 DEG C or 900-1000 DEG C at the speed of 5-15 DEG C/min, keeping the temperature for 40-80 min, raising the temperature to 1000-1500 DEG C or 1600-1800 DEG C at the speed of 5-15 DEG C/min, keeping the temperature for 2-8 h, cooling to the temperature of 300-400 DEG C at the speed of 18-25 DEG C/min, and cooling to the room temperature along with a furnace to obtain preliminary carbon; soaking: placing the preliminary carbon into a solution with acid content as 3-5wt%, soaking for 20-40 min, then soaking the carbon in a potassium oxalate solution with mass fraction as 8-10% according to the mass ratio as 1:3-4 for 3-5 h, and then washing with deionized water till pH of the carbon is neutral; microwave processing; and manufacturing the granule. The granule does not contain dust or impurities, is good in antistatic property and has a health care function.

Description

The dustless health carbon granule of a kind of conduction
technical field
The present invention relates to field of polymer technology, relate in particular to the dustless health carbon granule of a kind of conduction.
Background technology
At present, the method for firing carbo lignius material once charing is fired method and graded temperature-control is fired method.
It is that the carbo lignius of incomplete charing is carried out to the method that high temperature sintering is prepared conduction carbo lignius material again that method is fired in secondary charing.As Japanese Patent JP 2005035806 conduction charcoals or bamboo charcoal and preparation method thereof, be by the block charcoal after charing or bamboo charcoal upper 1000 ℃ with on once charing prepare the method for electroconductibility charcoal or bamboo charcoal.This preparation method's charcoal yield is higher, but sintering process needs secondary temperature elevation sintering, reduce, and have the inhomogeneous phenomenon of charing, so electric conductivity is difficult to improve thereby easily there is char combustion charcoal density in double sintering process.
It is in combustion processes that graded temperature-control is fired method; first furnace temperature is risen to sintering temperature; then cease fire and be cooled to lesser temps; blow-on is warming up to sintering temperature again; as Chinese patent ZL02129280.9 method of producing electric bamboo, be that bulk material is put into sintering oven, first furnace temperature is risen to 1500 ℃; then be cooled to 700 ℃, then rise to the method for 1500 ℃.This method charring process time is grown, yields poorly, and electric conductivity is not high.
Aforesaid method is block timber or bamboo wood carbonized, and is to be all warmed up to sintering temperature to lower the temperature immediately, therefore all has the features such as charing is inhomogeneous, poor stability, electric conductivity is low, static resistance is poor.And containing dust impurity, health-caring function haves much room for improvement.
Summary of the invention
The object of this invention is to provide a kind of dust and impurity, dustless health carbon granule of static resistance conduction good, that there is health-caring function of not containing.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
Conduct electricity a dustless health carbon granule, it is prepared from by following steps:
(1) raw material pre-treatment: plant material is sent in microwave vacuum tank, be evacuated to vacuum tightness for-0.02MPa~-0.001MPa, then carry out microwave treatment, microwave frequency is 300MHz~950MHz, and microwave treatment time is 1~3min;
(2) elementary charcoal preparation: the plant material through raw material pre-treatment gained is experienced to dry, pre-charing, charing, calcining and cooling successively, control combustion is warming up to 700-750 ℃ or 900-1000 ℃ and is incubated 40-80min with the speed of 5-15 ℃/min, and then be warming up to 1000-1500 ℃ or 1600-1800 ℃ and be incubated 2-8h with the speed of 5-15 ℃/min, then the speed with 18-25 ℃/min is cooled to 300-400 ℃, cool to again room temperature with the furnace, obtain elementary charcoal;
(3) immersion treatment: the solution of the elementary charcoal of gained being put into acid content 3-5wt% soaks 20-40min;
(4) then activation treatment: the Potassium Oxalate Solution that is 8-10% with massfraction by the particle after immersion treatment is 1:3-4 mixing submergence 3-5h is in mass ratio neutral by washed with de-ionized water to pH value;
(5) microwave treatment: step (4) gained material is carried out to microwave treatment, and microwave frequency is 500~650MHz, and microwave treatment time is 1~3min;
(6) carbon granule preparation.
Advantage of the present invention is:
1. by pre-treatment, can control moisture and the perforate of plant material, contribute to the preparation of follow-up elementary charcoal, can improve the conduction of elementary charcoal and de-taste function, the plant charcoal surface resistivity of preparation is high, there is good conductivity, the static resistance of carbon granule goods is had to promoter action;
2. this plant charcoal particle and having de-tastes and antibacterial, and dirt is had to adsorption, assists in removing the peculiar smell in environment; Be placed in water, can adsorbing chloride ions, the fine impurity such as tea stain, water is purified;
The carbon granule electric conductivity of 3. passing through immersion treatment is high, and not containing dust impurity, far infrared effect is good, can promote health insulation and peripheral blood circulation, has good health care function;
4. contriver finds to activate and microwave treatment after immersion treatment again, can strengthen the antibacterial ability of charcoal particle, and the negative ion releasing function of carbon granule of the present invention is improved, and can improve user's vital capacity, improves sleep quality.
As preferably, described step (1) plant material is corn cob, bamboo or pine tree.
More preferably, for corn cob or bamboo, control combustion is warming up to 700-750 ℃ and be incubated 40-80min with the speed of 5-15 ℃/min, and then be warming up to 1000-1500 ℃ and be incubated 2-8h with the speed of 5-15 ℃/min, then the speed with 20-23 ℃/min is cooled to 330-380 ℃, cool to again room temperature with the furnace, obtain elementary charcoal.
More preferably, for pine tree, control combustion is warming up to 900-1000 ℃ and be incubated 40-80min with the speed of 5-15 ℃/min, and then be warming up to 1600-1800 ℃ and be incubated 2-8h with the speed of 5-15 ℃/min, then the speed with 20-23 ℃/min is cooled to 330-380 ℃, cool to again room temperature with the furnace, obtain elementary charcoal.
As preferably, described step (1) is sent into plant material in microwave vacuum tank, is evacuated to vacuum tightness for-0.01MPa~-0.005MPa, then carries out microwave treatment, and microwave frequency is 300MHz~950MHz, and microwave treatment time is 1.2~2min.
As preferably, described step (3) immersion treatment is that the solution that the elementary charcoal of gained is put into acid content 3-5wt% soaks 30min.
More preferably, described solution is the acid solution containing 4wt%HCl.
More preferably, described solution is for containing H 2sO 4the sulphuric acid soln of amount 5wt%.
As preferably, the Potassium Oxalate Solution that described step (4) activation treatment is is 9% by the particle after immersion treatment with massfraction is 1:3.5 mixing submergence 4h in mass ratio, by washed with de-ionized water to pH value, is then neutral.
As preferably, described step (5) microwave treatment is that gained material is carried out to microwave treatment, and microwave frequency is 550~600MHz, and microwave treatment time is 1.2~2min.
As preferably, the preparation of described step (6) carbon granule is that the material after microwave treatment is made to the charcoal particle that diameter is 0.5-2mm with pulverizer or hydropress.
Accompanying drawing explanation
Fig. 1 is the temperature controlling system schematic diagram of the vertical moving-bed of plant charcoal charing of the present invention;
In figure, A-drying zone; The pre-char zone of B-; C-char zone; D-calcining zone; E-cooling zone; F-is with the temperature sensing device of CPU; D1/d2/d3-oxidizer entrance hole; T1/t2/t3-point for measuring temperature.
Embodiment
As shown in Figure 1, the vertical moving-bed that plant charcoal preparation is used is divided into drying zone A, pre-char zone B, char zone C, calcining zone D and cooling zone E.D mono-side in calcining zone is distributed with many oxidizer entrance holes that can regulate closure or openness, as d1, d2, d3 etc., opposite side is to having the point for measuring temperature at each aperture place as t1, t2, t3 etc., and each aperture place temperature shows by the temperature sensing device F being connected with this point for measuring temperature.
Embodiment mono-
The plant material that the present embodiment adopts is corn cob.
Plant material is sent in microwave vacuum tank, be evacuated to vacuum tightness for-0.02MPa, then carry out microwave treatment, microwave frequency is 300MHz, and microwave treatment time is 1min, plant material through pre-treatment gained is experienced dry successively, pre-charing, charing, calcining and cooling, the temperature of each point for measuring temperature, drying zone A is 150 ℃, pre-char zone B is 275 ℃, char zone C is 450 ℃, during intensification, observe the temperature of the district of D shown in Fig. 1 combustion zone different positions, when somewhere, combustion zone is as too low in the temperature of d2, open the aperture at this place, importing air locally burns, this place's temperature is raise, control the combustion zone temperature experiencing in bamboo folding process, control combustion is warming up to 700 ℃ and be incubated 40min with the speed of 5 ℃/min, and then be warming up to 1600 ℃ and be incubated 2h with the speed of 5 ℃/min,
Then the speed with 23-25 ℃/min is cooled to 380-400 ℃, then cools to room temperature with the furnace, obtains elementary charcoal; The solution that the elementary charcoal of gained is put into containing HNO3 amount 3-5wt% soaks 20min, then the Potassium Oxalate Solution that is 10% with massfraction by the particle after immersion treatment 1:4 mixing submergence 5h in mass ratio, by washed with de-ionized water to pH value, is then neutrality;
And then carry out microwave treatment, and microwave frequency is 600~650MHz, microwave treatment time is 2~3min; Finally with pulverizer or hydropress, make the charcoal particle that diameter is 0.5-2mm.
Detect performance in Table 1.The iodine sorption value of measuring carbon granule according to GB GB/T12496.10 is to react its absorption property.
Embodiment bis-
The plant material that the present embodiment adopts is bamboo chip (being about 40cm).
Plant material is sent in microwave vacuum tank, be evacuated to vacuum tightness for-0.001MPa, then carry out microwave treatment, microwave frequency is 950MHz, and microwave treatment time is 3min;
Plant material through pre-treatment gained is experienced dry successively, pre-charing, charing, calcining and cooling, the temperature of each point for measuring temperature, drying zone A is 150 ℃, pre-char zone B is 275 ℃, char zone C is 450 ℃, during intensification, observe the temperature of the district of D shown in Fig. 1 combustion zone different positions, when somewhere, combustion zone is as too low in the temperature of d2, open the aperture at this place, importing air locally burns, this place's temperature is raise, control the combustion zone temperature experiencing in bamboo folding process, control combustion is warming up to 750 ℃ and be incubated 80min with the speed of 15 ℃/min, and then heat up 1500 ℃ and be incubated 8h with the speed of 15 ℃/min,
Then the speed with 18-23 ℃/min is cooled to 300-330 ℃, then cools to room temperature with the furnace, obtains elementary charcoal; The elementary charcoal of gained is put into containing H 2sO 4in the sulphuric acid soln of amount 5wt%, soak 40min, then the Potassium Oxalate Solution that is 8% with massfraction by the particle after immersion treatment 1:3 mixing submergence 3h in mass ratio, by washed with de-ionized water to pH value, be then neutrality;
And then carry out microwave treatment, and microwave frequency is 500~550MHz, microwave treatment time is 1~1.2min; Finally with pulverizer, make the charcoal particle that diameter is 0.5-2mm.
Embodiment tri-
The plant material that the present embodiment adopts is pine tree, ingresses after pine tree is removed to epidermis impurity, and length is controlled and is no more than 15cm.
Plant material is sent in microwave vacuum tank, and being evacuated to vacuum tightness is-0.01~-0.005MPa, then carries out microwave treatment, and microwave frequency is 550MHz, and microwave treatment time is 1.2-2min;
Plant material through pre-treatment gained is experienced dry successively, pre-charing, charing, calcining and cooling, the temperature of each point for measuring temperature, drying zone A is 180 ℃, pre-char zone B is 325 ℃, char zone C is 530 ℃, during intensification, observe the temperature of the district of D shown in Fig. 1 combustion zone different positions, when somewhere, combustion zone is as too low in the temperature of d2, open the aperture at this place, importing air locally burns, this place's temperature is raise, control the combustion zone temperature experiencing in bamboo folding process, control combustion is warming up to 900 ℃ and be incubated 50min with the speed of 10 ℃/min, and then be warming up to 1600 ℃ and be incubated 5h with the speed of 10 ℃/min,
Then the speed with 20-23 ℃/min is cooled to 330-380 ℃, then cools to room temperature with the furnace, obtains elementary charcoal; The hydrochloric acid soln that the elementary charcoal of gained is put into containing HCl amount 4wt% soaks 30min, then the Potassium Oxalate Solution that is 9% with massfraction by the particle after immersion treatment 1:3.5 mixing submergence 4h in mass ratio, by washed with de-ionized water to pH value, is then neutrality;
And then carry out microwave treatment, and microwave frequency is 550~600MHz, microwave treatment time is 1.2~2min; Finally with hydropress, make the charcoal particle that diameter is 0.5-2mm.
Embodiment tetra-
With embodiment tri-, different is that the raw material using is beech; Control combustion is warming up to 1000 ℃ and be incubated 50min with the speed of 10 ℃/min, and then is warming up to 1800 ℃ and be incubated 5h with the speed of 10 ℃/min.
Comparative example one
With embodiment mono-, different is that plant material does not pass through microwave vacuum pre-treatment, but after being directly prepared into elementary charcoal, again prepared by immersion treatment, microwave treatment and carbon granule.
Comparative example two
With embodiment mono-, different is that elementary charcoal does not carry out immersion treatment after preparation, but directly carries out microwave treatment and carbon granule preparation.
Comparative example three
With embodiment tri-, different is not carry out activation treatment and microwave treatment after immersion treatment, but directly with being placed on after deionized water wash after drying in air, carries out carbon granule preparation.
Each embodiment of table 1 and comparative example's product performance index
As can be seen from Table 1,
(1) surface resistivity of the embodiment of the present invention one-embodiment four-product is little, and its good conductivity is described, its antistatic property is strong; The plant material that embodiment tetra-adopts is beech, and its various aspects of performance is slightly poor;
(2) comparative example one has omitted a certain step in preparation method of the present invention to comparative example three, and the various aspects of performance of its product is poor.
This specific embodiment is only explanation of the invention; it is not limitation of the present invention; those skilled in the art can make to the present embodiment the modification that there is no creative contribution as required after reading this specification sheets, but as long as within the scope of claim of the present invention, are all subject to the protection of patent law.

Claims (7)

  1. Conduction a dustless health carbon granule, it is characterized in that: it is prepared from by following steps:
    (1) raw material pre-treatment: plant material is sent in microwave vacuum tank, be evacuated to vacuum tightness for-0.02MPa~-0.001MPa, then carry out microwave treatment, microwave frequency is 300MHz~950MHz, and microwave treatment time is 1~3min;
    Described plant material is corn cob, bamboo or pine tree;
    (2) elementary charcoal preparation: the plant material through raw material pre-treatment gained is experienced to dry, pre-charing, charing, calcining and cooling successively;
    For corn cob or bamboo, control combustion is warming up to 700-750 ℃ and be incubated 40-80min with the speed of 5-15 ℃/min, and then be warming up to 1000-1500 ℃ and be incubated 2-8h with the speed of 5-15 ℃/min, then the speed with 20-23 ℃/min is cooled to 330-380 ℃, cool to again room temperature with the furnace, obtain elementary charcoal;
    For pine tree, control combustion is warming up to 900-1000 ℃ and be incubated 40-80min with the speed of 5-15 ℃/min, and then be warming up to 1600-1800 ℃ and be incubated 2-8h with the speed of 5-15 ℃/min, then the speed with 20-23 ℃/min is cooled to 330-380 ℃, cool to again room temperature with the furnace, obtain elementary charcoal;
    (3) immersion treatment: the solution of the elementary charcoal of gained being put into acid content 3-5wt% soaks 20-40min;
    (4) then activation treatment: the Potassium Oxalate Solution that is 8-10% with massfraction by the particle after immersion treatment is 1:3-4 mixing submergence 3-5h is in mass ratio neutral by washed with de-ionized water to pH value;
    (5) microwave treatment: step (4) gained material is carried out to microwave treatment, and microwave frequency is 500~650MHz, and microwave treatment time is 1~3min;
    (6) carbon granule preparation.
  2. 2. the dustless health carbon granule of a kind of conduction according to claim 1, it is characterized in that: described step (1) is sent into plant material in microwave vacuum tank, being evacuated to vacuum tightness is-0.01MPa~-0.005MPa, carry out again microwave treatment, microwave frequency is 300MHz~950MHz, and microwave treatment time is 1.2~2min.
  3. 3. the dustless health carbon granule of a kind of conduction according to claim 1, is characterized in that: described step (3) immersion treatment is that the solution that the elementary charcoal of gained is put into acid content 3-5wt% soaks 30min.
  4. 4. the dustless health carbon granule of a kind of conduction according to claim 1, is characterized in that: the solution of described acid content 3-5wt% is the acid solution containing 4wt%HCl.
  5. 5. the dustless health carbon granule of a kind of conduction according to claim 1, it is characterized in that: the Potassium Oxalate Solution that described step (4) activation treatment is is 9% by the particle after immersion treatment with massfraction is 1:3.5 mixing submergence 4h in mass ratio, is then neutral by washed with de-ionized water to pH value.
  6. 6. the dustless health carbon granule of a kind of conduction according to claim 1, is characterized in that: described step (5) microwave treatment is that gained material is carried out to microwave treatment, and microwave frequency is 550~600MHz, and microwave treatment time is 1.2~2min.
  7. 7. according to the dustless health carbon granule of a kind of conduction described in claim 3-6 any one, it is characterized in that: the preparation of described step (6) carbon granule is that the material after microwave treatment is made to the charcoal particle that diameter is 0.5-2mm with pulverizer or hydropress.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1736859A (en) * 2005-08-15 2006-02-22 昆明理工大学 Super active carbon preparation method
EP1786008A1 (en) * 2004-08-18 2007-05-16 Nippon Oil Corporation Raw material carbon composition for carbon material for electrode of electric double layer capacitor
CN1986399A (en) * 2006-12-25 2007-06-27 天津城市建设学院 Preparing process of active sludge carbon for desulfurizing fume
CN101092238A (en) * 2007-06-08 2007-12-26 山东大学 Method for preparing active carbon of typha and calamus
CN101717084A (en) * 2009-12-09 2010-06-02 昆明理工大学 Method for preparing mesoporous activated carbon from shell of jatropha curcas
CN102092711A (en) * 2011-01-13 2011-06-15 山东大学 Method for preparing activated carbon from Chinese medicinal dregs
CN102275917A (en) * 2011-07-26 2011-12-14 福建农林大学 Preparation method of high-specific surface area mangosteen shell active carbon rich in mesopores

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1786008A1 (en) * 2004-08-18 2007-05-16 Nippon Oil Corporation Raw material carbon composition for carbon material for electrode of electric double layer capacitor
CN1736859A (en) * 2005-08-15 2006-02-22 昆明理工大学 Super active carbon preparation method
CN1986399A (en) * 2006-12-25 2007-06-27 天津城市建设学院 Preparing process of active sludge carbon for desulfurizing fume
CN101092238A (en) * 2007-06-08 2007-12-26 山东大学 Method for preparing active carbon of typha and calamus
CN101717084A (en) * 2009-12-09 2010-06-02 昆明理工大学 Method for preparing mesoporous activated carbon from shell of jatropha curcas
CN102092711A (en) * 2011-01-13 2011-06-15 山东大学 Method for preparing activated carbon from Chinese medicinal dregs
CN102275917A (en) * 2011-07-26 2011-12-14 福建农林大学 Preparation method of high-specific surface area mangosteen shell active carbon rich in mesopores

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