CN112079353A - Preparation technology of active biochar for modifying traditional Chinese medicine residues - Google Patents
Preparation technology of active biochar for modifying traditional Chinese medicine residues Download PDFInfo
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- CN112079353A CN112079353A CN202010918431.1A CN202010918431A CN112079353A CN 112079353 A CN112079353 A CN 112079353A CN 202010918431 A CN202010918431 A CN 202010918431A CN 112079353 A CN112079353 A CN 112079353A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C01B32/342—Preparation characterised by non-gaseous activating agents
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Abstract
The invention discloses a preparation technology of traditional Chinese medicine residue modified activated charcoal, belonging to the technical field of preparation of traditional Chinese medicine residue modified activated charcoal, wherein the preparation technology of the activated charcoal comprises the specific steps of raw material pretreatment, activating agent treatment, activation carbonization, washing, drying, grinding and sieving to obtain the traditional Chinese medicine residue activated charcoal, and the prepared traditional Chinese medicine residue activated charcoal is prepared according to the ratio of 10g of activated charcoal to 100mL (the concentration is 6mol/L) of HNO3The solutions are mixed, boiled for 60min together, cooled and filtered, then repeatedly washed by distilled water until the conductivity of the filtrate reaches below 3uS/cm, then the mixture is dried to constant weight and fully crushed to obtain the modified traditional Chinese medicine residue activated carbon, which can increase new sources of activated carbon preparation, simultaneously does not need to add redundant raw materials, has low production cost, can realize resource utilization of waste, can greatly improve the adsorption capacity of the activated carbon through modification treatment of a strong oxidant, enhances the adsorption effect and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of preparation of traditional Chinese medicine residue modified activated charcoal, in particular to a preparation technology of traditional Chinese medicine residue modified activated charcoal.
Background
The traditional Chinese medicine dregs are mainly derived from Chinese patent medicine production, raw material medicine production, traditional Chinese medicine processing and concocting, light chemical product production containing traditional Chinese medicines and the like, and the quantity of the dregs brought by the Chinese patent medicine production is the largest and accounts for about 70 percent of the total quantity of the dregs. The traditional Chinese medicine residues are typical industries and have the characteristics of complex shapes, high water content and the like, the traditional Chinese medicine residues are byproducts generated in the processes of production of raw medicines, production of Chinese patent medicines, processing and concocting of traditional Chinese medicines and production of light chemical products containing traditional Chinese medicines, the residues are rich in organic substances such as fibers, polysaccharides, proteins and the like, nitrogen, phosphorus, potassium and trace elements and contain a certain amount of active ingredients, the plant medicine residue fermentation residues contain unutilized cellulose and undegraded lignin, the lignin contains carbon by more than 50 percent and is a suitable raw material for producing carbon materials, the active carbon can be prepared, the fermentation residues are used for preparing the active carbon, new sources for preparing the active carbon can be increased, theoretical support is provided for resource utilization of wastes, and the preparation technology is environment-friendly and energy-saving.
Disclosure of Invention
The invention aims to provide a preparation technology of active biochar for modifying traditional Chinese medicine residues, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a technology for preparing active biochar for modifying traditional Chinese medicine residues comprises the following specific steps:
the method comprises the following steps: pretreatment of raw materials: cleaning the raw materials of the traditional Chinese medicine residues, placing the raw materials in a stainless steel drying box, keeping the temperature in the stainless steel drying box between 75 and 90 ℃, keeping the temperature for drying for 60 to 72 hours, then transferring the raw materials into a dryer, cooling the raw materials for 24 hours, crushing the raw materials by a crusher, and sieving the crushed raw materials by a 100-mesh sieve for later use;
step two: and (3) activating agent treatment: a phosphoric acid solution having a concentration of 35% was mixed at an impregnation ratio (ratio of the mass of the solid to the mass of the liquid) of 1: 3, mixing the mixture with the Chinese medicine residues treated in the previous step, uniformly mixing, soaking for 48 hours, and performing solid-liquid separation by using a vacuum filtering device after the soaking is finished;
step three: activating and carbonizing: filtering the traditional Chinese medicine residue mixture subjected to the dipping treatment in the previous step, then putting the traditional Chinese medicine residue mixture into a stainless steel drying oven for drying, keeping the temperature in the stainless steel drying oven between 75 and 90 ℃, drying until the water content is less than 15 percent, keeping the drying time for 48 to 72 hours, taking out the traditional Chinese medicine residue mixture after the drying is finished, then wrapping the dried material residue with tinfoil, putting the wrapped material residue into a muffle furnace, and carbonizing the material residue at the constant temperature of 400 ℃ for 30 to 40 minutes;
step four: washing: naturally cooling the carbonized Chinese medicinal residue to room temperature, taking out, repeatedly washing with distilled water, and washing thoroughly until pH value is 6.5-7.5;
step five: and (3) drying: placing the washed carbonized traditional Chinese medicine residues into a stainless steel drying box for drying, keeping the temperature in the stainless steel drying box between 100 ℃ and 120 ℃, drying until the water content is less than 5 percent, keeping the drying time to be more than 48 percent, taking out the carbonized traditional Chinese medicine residues, placing the carbonized traditional Chinese medicine residues into a dryer, cooling the carbonized traditional Chinese medicine residues for 24 hours, and then, keeping the weight of the product;
step six: grinding and sieving: grinding the product obtained in the last step in a mortar, then sieving the ground product with a 200-mesh sieve, and bottling the sieved material for later use to obtain the traditional Chinese medicine residue activated carbon;
step seven: mixing the prepared traditional Chinese medicine residue activated carbon with 100mL (6 mol/L) of HNO according to the ratio of 10g activated carbon to 100mL3Mixing the above solutions, boiling for 60min, cooling, filtering, repeatedly washing with distilled water until the conductivity of the filtrate reaches below 3uS/cm, drying the mixture to constant weight, and pulverizing to obtain modified Chinese medicinal residue activated carbon.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of cleaning and crushing the traditional Chinese medicine residues, activating the crushed traditional Chinese medicine residues, carbonizing the crushed traditional Chinese medicine residues in a muffle furnace at a constant temperature, washing, drying, grinding and sieving the carbonized traditional Chinese medicine residues to finish the preparation of the traditional Chinese medicine residue activated carbon, adding a new source for preparing the activated carbon by using the traditional Chinese medicine residues as raw materials, simultaneously adding no redundant raw materials, having low production cost, not generating waste gas and waste liquid polluting the environment in the preparation process, protecting the environment, saving energy, realizing the resource utilization of wastes, and obviously increasing the specific surface area and the micropore volume and lengthening the average pore diameter of the traditional Chinese medicine residue activated carbon subjected to nitric acid modification. The specific surface area reaches 161.798m2The volume of the pores reaches 121.374m2(ii)/g, 30 times that of unmodified activated carbon; the average pore diameter reaches 24.209m2Per g, an increase of approximately 6-fold. The adsorption energy of the active carbon can be greatly improved by modification treatment with strong oxidantThe adsorption effect is enhanced, and the method has wide application prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A technology for preparing active biochar for modifying traditional Chinese medicine residues comprises the following specific steps:
the method comprises the following steps: pretreatment of raw materials: cleaning the raw materials of the traditional Chinese medicine residues, placing the raw materials in a stainless steel drying box, keeping the temperature in the stainless steel drying box at 90 ℃, keeping the temperature for drying for 60 hours, then transferring the raw materials into a dryer, cooling the raw materials for 24 hours, crushing the raw materials by using a crusher, and sieving the crushed raw materials by using a 100-mesh sieve for later use;
step two: and (3) activating agent treatment: a phosphoric acid solution having a concentration of 35% was mixed at an impregnation ratio (ratio of the mass of the solid to the mass of the liquid) of 1: 3, mixing the mixture with the Chinese medicine residues treated in the previous step, uniformly mixing, soaking for 48 hours, and performing solid-liquid separation by using a vacuum filtering device after the soaking is finished;
step three: activating and carbonizing: filtering the traditional Chinese medicine residue mixture subjected to the dipping treatment in the previous step, then placing the mixture into a stainless steel drying oven for drying, keeping the temperature in the stainless steel drying oven at 90 ℃, drying until the water content is less than 15%, continuously drying for 48 hours, taking out the mixture after the drying is finished, then wrapping the dried material residue with tinfoil, placing the wrapped material residue into a muffle furnace, and carbonizing the wrapped material residue at the constant temperature of 400 ℃ for 30 min;
step four: washing: naturally cooling the carbonized Chinese medicinal residue to room temperature, taking out, repeatedly washing with distilled water, and washing thoroughly until pH value is 6.5-7.5;
step five: and (3) drying: placing the washed carbonized traditional Chinese medicine residues into a stainless steel drying oven for drying, keeping the temperature in the stainless steel drying oven at 120 ℃, drying until the water content is less than 5%, and continuously drying for more than 48%, taking out the carbonized traditional Chinese medicine residues and placing the carbonized traditional Chinese medicine residues into a dryer for cooling for 24 hours, and then, keeping the weight of the product;
step six: grinding and sieving: grinding the product obtained in the last step in a mortar, then sieving the ground product with a 200-mesh sieve, and bottling the sieved material for later use to obtain the traditional Chinese medicine residue activated carbon;
step seven: mixing the prepared traditional Chinese medicine residue activated carbon with 100mL (6 mol/L) of HNO according to the ratio of 10g activated carbon to 100mL3Mixing the above solutions, boiling for 60min, cooling, filtering, repeatedly washing with distilled water until the conductivity of the filtrate reaches below 3uS/cm, drying the mixture to constant weight, and pulverizing to obtain modified Chinese medicinal residue activated carbon.
Example 2
A technology for preparing active biochar for modifying traditional Chinese medicine residues comprises the following specific steps:
the method comprises the following steps: pretreatment of raw materials: cleaning the raw materials of the traditional Chinese medicine residues, placing the raw materials in a stainless steel drying box, keeping the temperature in the stainless steel drying box at 75 ℃, keeping the temperature for drying for 72 hours, then transferring the raw materials into a dryer, cooling the raw materials for 24 hours, crushing the raw materials by using a crusher, and sieving the crushed raw materials by using a 100-mesh sieve for later use;
step two: and (3) activating agent treatment: a phosphoric acid solution having a concentration of 35% was mixed at an impregnation ratio (ratio of the mass of the solid to the mass of the liquid) of 1: 3, mixing the mixture with the Chinese medicine residues treated in the previous step, uniformly mixing, soaking for 48 hours, and performing solid-liquid separation by using a vacuum filtering device after the soaking is finished;
step three: activating and carbonizing: filtering the traditional Chinese medicine residue mixture subjected to the dipping treatment in the previous step, then placing the mixture into a stainless steel drying oven for drying, keeping the temperature in the stainless steel drying oven at 75 ℃, drying until the water content is less than 15%, continuously drying for 72 hours, taking out the mixture after the drying is finished, then wrapping the dried material residue with tinfoil, placing the wrapped material residue into a muffle furnace, and carbonizing the wrapped material residue at the constant temperature of 400 ℃ for 40 min;
step four: washing: naturally cooling the carbonized Chinese medicinal residue to room temperature, taking out, repeatedly washing with distilled water, and washing thoroughly until pH value is 6.5-7.5;
step five: and (3) drying: placing the washed carbonized traditional Chinese medicine residues into a stainless steel drying oven for drying, keeping the temperature in the stainless steel drying oven at 100 ℃, drying until the water content is less than 5%, and continuously drying for more than 48%, taking out the carbonized traditional Chinese medicine residues and placing the carbonized traditional Chinese medicine residues into a dryer for cooling for 24 hours, and then, keeping the weight of the product;
step six: grinding and sieving: grinding the product obtained in the last step in a mortar, then sieving the ground product with a 200-mesh sieve, and bottling the sieved material for later use to obtain the traditional Chinese medicine residue activated carbon;
step seven: mixing the prepared traditional Chinese medicine residue activated carbon with 100mL (6 mol/L) of HNO according to the ratio of 10g activated carbon to 100mL3Mixing the above solutions, boiling for 60min, cooling, filtering, repeatedly washing with distilled water until the conductivity of the filtrate reaches below 3uS/cm, drying the mixture to constant weight, and pulverizing to obtain modified Chinese medicinal residue activated carbon.
The method comprises the steps of cleaning and crushing traditional Chinese medicine residues, activating the crushed traditional Chinese medicine residues, carbonizing the crushed traditional Chinese medicine residues in a muffle furnace at a constant temperature, washing, drying, grinding and sieving the carbonized traditional Chinese medicine residues to finish the preparation of the traditional Chinese medicine residue activated carbon, using the traditional Chinese medicine residues as raw materials, increasing new sources for preparing the activated carbon, simultaneously not adding redundant raw materials, having low production cost, not generating waste gas and waste liquid polluting the environment in the preparation process, protecting the environment, saving energy, realizing the resource utilization of wastes, and obviously increasing the specific surface area and the micropore volume and lengthening the average pore diameter of the traditional Chinese medicine residue activated carbon subjected to nitric acid modification. The specific surface area reaches 161.798m2The volume of the pores reaches 121.374m2(ii)/g, 30 times that of unmodified activated carbon; the average pore diameter reaches 24.209m2Per g, an increase of approximately 6-fold. Can be greatly improved by modification treatment with strong oxidantHigh adsorption capacity of the active carbon, enhanced adsorption effect and wide application prospect.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A preparation technology of active biochar for modifying traditional Chinese medicine residues is characterized by comprising the following steps: the preparation method of the biochar comprises the following specific steps:
the method comprises the following steps: pretreatment of raw materials: cleaning the raw materials of the traditional Chinese medicine residues, placing the raw materials in a stainless steel drying box, keeping the temperature in the stainless steel drying box between 75 and 90 ℃, keeping the temperature for drying for 60 to 72 hours, then transferring the raw materials into a dryer, cooling the raw materials for 24 hours, crushing the raw materials by a crusher, and sieving the crushed raw materials by a 100-mesh sieve for later use;
step two: and (3) activating agent treatment: a phosphoric acid solution having a concentration of 35% was mixed at an impregnation ratio (ratio of the mass of the solid to the mass of the liquid) of 1: 3, mixing the mixture with the Chinese medicine residues treated in the previous step, uniformly mixing, soaking for 48 hours, and performing solid-liquid separation by using a vacuum filtering device after the soaking is finished;
step three: activating and carbonizing: filtering the traditional Chinese medicine residue mixture subjected to the dipping treatment in the previous step, then putting the traditional Chinese medicine residue mixture into a stainless steel drying oven for drying, keeping the temperature in the stainless steel drying oven between 75 and 90 ℃, drying until the water content is less than 15 percent, keeping the drying time for 48 to 72 hours, taking out the traditional Chinese medicine residue mixture after the drying is finished, then wrapping the dried material residue with tinfoil, putting the wrapped material residue into a muffle furnace, and carbonizing the material residue at the constant temperature of 400 ℃ for 30 to 40 minutes;
step four: washing: naturally cooling the carbonized Chinese medicinal residue to room temperature, taking out, repeatedly washing with distilled water, and washing thoroughly until pH value is 6.5-7.5;
step five: and (3) drying: placing the washed carbonized traditional Chinese medicine residues into a stainless steel drying box for drying, keeping the temperature in the stainless steel drying box between 100 ℃ and 120 ℃, drying until the water content is less than 5 percent, keeping the drying time to be more than 48 percent, taking out the carbonized traditional Chinese medicine residues, placing the carbonized traditional Chinese medicine residues into a dryer, cooling the carbonized traditional Chinese medicine residues for 24 hours, and then, keeping the weight of the product;
step six: grinding and sieving: grinding the product obtained in the last step in a mortar, then sieving the ground product with a 200-mesh sieve, and bottling the sieved material for later use to obtain the traditional Chinese medicine residue activated carbon;
step seven: mixing the prepared traditional Chinese medicine residue activated carbon with 100mL (6 mol/L) of HNO according to the ratio of 10g activated carbon to 100mL3Mixing the above solutions, boiling for 60min, cooling, filtering, repeatedly washing with distilled water until the conductivity of the filtrate reaches below 3uS/cm, drying the mixture to constant weight, and pulverizing to obtain modified Chinese medicinal residue activated carbon.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112940766A (en) * | 2021-02-23 | 2021-06-11 | 河北科技大学 | Streptomycin bacterium residue resource utilization method |
| CN113479876A (en) * | 2021-08-05 | 2021-10-08 | 河南中医药大学 | Belladonna herb residue porous carbon and preparation method and application thereof |
| CN114392717A (en) * | 2021-12-07 | 2022-04-26 | 河南省城乡水务研究院有限公司 | Traditional Chinese medicine residue biochar, preparation method and application |
| CN115353104A (en) * | 2022-09-05 | 2022-11-18 | 山西顺福祥环保科技有限责任公司 | Method for preparing columnar activated carbon by using traditional Chinese medicine residues and product |
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Application publication date: 20201215 |