CN102942174B - Manufacture method for electric conduction dust-free health care carbon granule - Google Patents
Manufacture method for electric conduction dust-free health care carbon granule Download PDFInfo
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- CN102942174B CN102942174B CN201210481537.5A CN201210481537A CN102942174B CN 102942174 B CN102942174 B CN 102942174B CN 201210481537 A CN201210481537 A CN 201210481537A CN 102942174 B CN102942174 B CN 102942174B
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Abstract
The invention relates to the field of macromolecules, in particular to a manufacture method for an electric conduction dust-free health care carbon granule. The method includes the following steps: pre-processing raw materials: placing plant raw materials into a microwave vacuum tank, vacuumizing to a vacuum degree as -0.002MPa to -0.001MPa, and conducting microwave processing; drying, pre-carbonizing, carbonizing, calcining and cooling the obtained plant raw materials after the pre-processing of the raw materials 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 mins, 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 washing with deionized water till pH of the carbon is neutral; microwave processing: conducting microwave processing on substances obtained in the step (3); and manufacturing the granule. The granule obtained through the method does not contain dust or impurities, is good in antistatic property and has a health care function.
Description
Technical field
The present invention relates to field of polymer technology, relate in particular to a kind of making method of conducting electricity dustless health carbon granule.
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 conducts electricity charcoal or bamboo charcoal and preparation method thereof, be by the block charcoal after charing or bamboo charcoal upper 1000 DEG C 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, reduces, and have the inhomogeneous phenomenon of charing thereby easily there is char combustion charcoal density in double sintering process, and therefore electric conductivity is difficult to improve.
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 mono-kind of Chinese patent ZL02129280.9 produces the method for electric bamboo, be that bulk material is put into sintering oven, first furnace temperature is risen to 1500 DEG C; then be cooled to 700 DEG C, then rise to the method for 1500 DEG C.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 making method that does not contain dust and impurity, the dustless health carbon granule of static resistance conduction good, that there is health-caring function.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
Conduct electricity the making method of dustless health carbon granule, it comprises the following steps successively:
(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: will experience successively dry, pre-charing, charing, calcining and cooling through the plant material of raw material pre-treatment gained, control combustion is warming up to 700-750 DEG C or 900-1000 DEG C and is incubated 40-80min with the speed of 5-15 DEG C/min, and then be warming up to 1000-1500 DEG C or 1600-1800 DEG C and be incubated 2-8h with the speed of 5-15 DEG C/min, then be cooled to 300-400 DEG C with the speed of 18-25 DEG C/min, cool to again room temperature with the furnace, obtain elementary charcoal;
(3) then immersion treatment: the solution that elementary gained charcoal is put into acid content 3-5wt% soaks 20-40min is neutral by washed with de-ionized water to pH value;
(4) microwave treatment: step (3) gained material is carried out to microwave treatment, and microwave frequency is 500~650MHz, and microwave treatment time is 1~3min;
(5) carbon granule preparation.
The advantage of the inventive method is:
1. can control moisture and the perforate of plant material by pre-treatment, 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 after immersion treatment, to carry out microwave 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 DEG C and be incubated 40-80min with the speed of 5-15 DEG C/min, and then be warming up to 1000-1500 DEG C and be incubated 2-8h with the speed of 5-15 DEG C/min, then be cooled to 330-380 DEG C with the speed of 20-23 DEG C/min, cool to again room temperature with the furnace, obtain elementary charcoal.
More preferably, for pine tree, control combustion is warming up to 900-1000 DEG C and be incubated 40-80min with the speed of 5-15 DEG C/min, and then be warming up to 1600-1800 DEG C and be incubated 2-8h with the speed of 5-15 DEG C/min, then be cooled to 330-380 DEG C with the speed of 20-23 DEG C/min, 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 elementary gained charcoal is put into acid content 3-5wt% soaks 30min, is then neutral by washed with de-ionized water to pH value.
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, described step (4) 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 (5) carbon granule is that the pulverizer of the material after microwave treatment or hydropress are made to the charcoal particle that diameter is 0.5-2mm.
Brief description of the drawings
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; The temperature sensing device of F-with 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, to experience successively dry through the plant material of pre-treatment gained, pre-charing, charing, calcining and cooling, the temperature of each point for measuring temperature, drying zone A is 150 DEG C, pre-char zone B is 275 DEG C, char zone C is 450 DEG C, when intensification, observe the temperature of the district of D shown in Fig. 1 combustion zone different positions, in the time that 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 DEG C and be incubated 40min with the speed of 5 DEG C/min, and then be warming up to 1600 DEG C and be incubated 2h with the speed of 5 DEG C/min,
Then be cooled to 380-400 DEG C with the speed of 23-25 DEG C/min, then cool to room temperature with the furnace, obtain elementary charcoal; Elementary gained charcoal is put into containing the solution of HNO3 amount 3-5wt% and soaked 20min, is then neutral by washed with de-ionized water to pH value;
And then carry out microwave treatment, and microwave frequency is 600~650MHz, microwave treatment time is 2~3min; Finally make with pulverizer or hydropress 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;
To experience successively dry through the plant material of pre-treatment gained, pre-charing, charing, calcining and cooling, the temperature of each point for measuring temperature, drying zone A is 150 DEG C, pre-char zone B is 275 DEG C, char zone C is 450 DEG C, when intensification, observe the temperature of the district of D shown in Fig. 1 combustion zone different positions, in the time that 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 DEG C and be incubated 80min with the speed of 15 DEG C/min, and then heat up 1500 DEG C and be incubated 8h with the speed of 15 DEG C/min,
Then be cooled to 300-330 DEG C with the speed of 18-23 DEG C/min, then cool to room temperature with the furnace, obtain elementary charcoal; Elementary gained charcoal is put into containing H
2sO
4in the sulphuric acid soln of amount 5wt%, soaking 40min, is then neutral by washed with de-ionized water to pH value;
And then carry out microwave treatment, and microwave frequency is 500~550MHz, microwave treatment time is 1~1.2min; Finally make with pulverizer 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 control 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;
To experience successively dry through the plant material of pre-treatment gained, pre-charing, charing, calcining and cooling, the temperature of each point for measuring temperature, drying zone A is 180 DEG C, pre-char zone B is 325 DEG C, char zone C is 530 DEG C, when intensification, observe the temperature of the district of D shown in Fig. 1 combustion zone different positions, in the time that 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 DEG C and be incubated 50min with the speed of 10 DEG C/min, and then be warming up to 1600 DEG C and be incubated 5h with the speed of 10 DEG C/min,
Then be cooled to 330-380 DEG C with the speed of 20-23 DEG C/min, then cool to room temperature with the furnace, obtain elementary charcoal; Elementary gained charcoal is put into containing the hydrochloric acid soln of HCl amount 4wt% and soaked 30min, is then neutral by washed with de-ionized water to pH value;
And then carry out microwave treatment, and microwave frequency is 550~600MHz, microwave treatment time is 1.2~2min; Finally make with hydropress 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 DEG C and be incubated 50min with the speed of 10 DEG C/min, and then is warming up to 1800 DEG C and be incubated 5h with the speed of 10 DEG C/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 microwave treatment after immersion treatment, carries out carbon granule preparation but be placed directly in after drying in air.
The 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 are reading after this specification sheets and can make to the present embodiment the amendment that there is no creative contribution as required, 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. a making method for the dustless health carbon granule of conduction, is characterized in that: comprise the following steps successively:
(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: will experience successively dry, pre-charing, charing, calcining and cooling through the plant material of raw material pre-treatment gained;
For corn cob or bamboo, control combustion is warming up to 700-750 DEG C and be incubated 40-80min with the speed of 5-15 DEG C/min, and then be warming up to 1000-1500 DEG C and be incubated 2-8h with the speed of 5-15 DEG C/min, then be cooled to 330-380 DEG C with the speed of 20-23 DEG C/min, cool to again room temperature with the furnace, obtain elementary charcoal;
For pine tree, control combustion is warming up to 900-1000 DEG C and be incubated 40-80min with the speed of 5-15 DEG C/min, and then be warming up to 1600-1800 DEG C and be incubated 2-8h with the speed of 5-15 DEG C/min, then be cooled to 330-380 DEG C with the speed of 20-23 DEG C/min, cool to again room temperature with the furnace, obtain elementary charcoal;
(3) then immersion treatment: the solution that elementary gained charcoal is put into acid content 3-5wt% soaks 20-40min is neutral by washed with de-ionized water to pH value;
(4) microwave treatment: step (3) gained material is carried out to microwave treatment, and microwave frequency is 500~650MHz, and microwave treatment time is 1~3min;
(5) carbon granule preparation.
2. a kind of making method of conducting electricity dustless health carbon granule 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. a kind of making method of conducting electricity dustless health carbon granule according to claim 2, it is characterized in that: described step (3) immersion treatment is that the solution that elementary gained charcoal is put into acid content 3-5wt% soaks 30min, is then neutral by washed with de-ionized water to pH value.
4. a kind of making method of conducting electricity dustless health carbon granule according to claim 3, is characterized in that: described solution is the acid solution containing 4wt%HCl.
5. a kind of making method of conducting electricity dustless health carbon granule according to claim 3, is characterized in that: described solution is for containing H
2sO
4the sulphuric acid soln of amount 5wt%.
6. a kind of making method of conducting electricity dustless health carbon granule according to claim 3, is characterized in that: described step (4) 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. a kind of making method of conducting electricity dustless health carbon granule according to claim 3, is characterized in that: the preparation of described step (5) carbon granule is that the pulverizer of the material after microwave treatment or hydropress are made to the charcoal particle that diameter is 0.5-2mm.
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JP2005035806A (en) * | 2003-07-15 | 2005-02-10 | Kyogyo Kumiai Hachiman Kawara Seisakusho | Conductive wood and bamboo charcoal and method of manufacturing conductive wood and bamboo charcoal |
JP2005281116A (en) * | 2004-03-31 | 2005-10-13 | Kochi Univ Of Technology | Method for producing activated carbon using microwave |
CN101921604B (en) * | 2010-08-30 | 2012-08-22 | 浙江建中竹业科技有限公司 | Dry distillation charring method for bamboos |
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Non-Patent Citations (2)
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