CN110193346A - Craboraffin preparation and preparation method thereof - Google Patents

Craboraffin preparation and preparation method thereof Download PDF

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Publication number
CN110193346A
CN110193346A CN201910466607.1A CN201910466607A CN110193346A CN 110193346 A CN110193346 A CN 110193346A CN 201910466607 A CN201910466607 A CN 201910466607A CN 110193346 A CN110193346 A CN 110193346A
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CN
China
Prior art keywords
raw material
preparation
charcoaid
catalyst
activation
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Pending
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CN201910466607.1A
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Chinese (zh)
Inventor
李正元
李菁
石志浩
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JIANGSU ZHUHAI ACTIVATED CARBON Co Ltd
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JIANGSU ZHUHAI ACTIVATED CARBON Co Ltd
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Priority to CN201910466607.1A priority Critical patent/CN110193346A/en
Publication of CN110193346A publication Critical patent/CN110193346A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention belongs to active carbon preparation fields, and in particular to a kind of craboraffin preparation and preparation method thereof.Wherein this preparation method includes: pretreatment of raw material, i.e., after raw material being passed through alkaline solution, then is impregnated in catalyst;Vacuum carburization processing, i.e., carry out microwave carbonization for raw material under vacuum conditions;Washing;And drying, the CharcoAid is made.From raw material and carbonization environment strict control, the adsorbance of foreign gas in CharcoAid is sufficiently lowered, improves the adsorption effect to pigment in liquid glucose.

Description

Craboraffin preparation and preparation method thereof
Technical field
The present invention relates to active carbon preparation fields, and in particular to a kind of craboraffin preparation and preparation method thereof.
Background technique
Major part sugar refinery in China's is all made of sulfurous method sugaring at present, and the generally existing color value of white sand sugar product is higher, dioxy Change the higher problem of sulfur content, is unable to reach international standard, the market competitiveness is weak.Existing CharcoAid is in preparation process In, purified treatment is not done to raw material, also not to environment vacuum is prepared, active carbon particle is caused to be easy absorption during the preparation process A large amount of impurity, such as: dust, suspended matter, sour gas etc. reduce active carbon particle to the adsorption effect of pigment in liquid glucose.
Summary of the invention
The object of the present invention is to provide a kind of craboraffin preparations and preparation method thereof.
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparation methods of CharcoAid, comprising: raw material is pre- Processing after raw material is passed through alkaline solution, then is impregnated in catalyst;Carbonization treatment, i.e., by raw material under vacuum conditions into The carbonization of row microwave;Washing;And drying, the CharcoAid is made.
Further, the mass ratio of the raw material and catalyst is 1:4-7.
Further, the catalyst includes: zinc chloride, HCl and water;Wherein chlorination zinc concentration is 55-75wt%;Catalysis The pH value of agent is 2.5-4.5.
Further, the method for the vacuum carburization processing includes: that raw material is put into vacuum drying oven, and vacuumizes;Heating is dry It is dry;Microwave carbonization;And heating activation.
Further, the temperature of the heat drying is 250-300 DEG C, drying time 20-50min.
Further, the power 400-550W of the microwave, radiated time 20-30min.
Further, the temperature of the heating activation is 850-1000 DEG C, activation time 100-150min.
Further, the raw material is wooden clast, and partial size is 200-500 mesh.
Another aspect, the present invention also provides a kind of CharcoAid, the CharcoAid is suitable under vacuum conditions Preparation.
The invention has the advantages that preparation method of the invention purifies raw material by alkaline solution, then urged Agent catalysis, then under vacuum conditions carry out microwave carbonization, finally by washing and drying and etc. prepare craboraffin system Agent sufficiently lowers the adsorbance of foreign gas in CharcoAid, improves to sugar from raw material and carbonization environment strict control The adsorption effect of pigment in liquid.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the process flow chart of preparation method of the invention.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with Illustration illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
Embodiment 1
As shown in Figure 1, the present embodiment 1 provides a kind of preparation method of CharcoAid, include the following steps: step S1, it is former Material pretreatment, i.e., after raw material being passed through alkaline solution, then be impregnated in catalyst;Step S2, carbonization treatment, i.e., by raw material true Microwave carbonization is carried out under Altitude;Step S3, washing;And the CharcoAid is made in step S4, drying.
Optionally, the alkaline solution is such as, but not limited to the solution such as sodium hydroxide, potassium hydroxide, calcium hydroxide, to remove The gases such as sulfur dioxide, hydrogen sulfide, the carbon dioxide in raw material are removed, catharsis is played, reduce the foreign gas in raw material.
Optionally, the raw material is wooden clast, and partial size is 200-500 mesh, is chosen as 300 mesh, 400 mesh.Raw material More thinner, easier progress carbonization-activation processing, total specific surface and burn tinctuer increase granularity, and the granularity of especially reduction raw material can subtract The quantity of aperture increases the ratio of mesoporous or macropore, the pigment etc. being more advantageous in absorption liquid glucose.
Optionally, the mass ratio of the raw material and catalyst is 1:4-7, is chosen as 1:5 or 1:6.5.
The preparation method of the present embodiment 1 purifies raw material by alkaline solution, then carries out catalyst, then in vacuum Under environment carry out microwave carbonization, finally by washing and drying and etc. prepare craboraffin preparation, original can be effectively reduced Impurity in material improves the adsorption effect to pigment in liquid glucose.
A kind of optional embodiment as catalyst.
The catalyst includes: zinc chloride, HCl and water;Wherein chlorination zinc concentration is 55-75wt%, is chosen as 60wt%; The pH value of catalyst is 2.5-4.5, and being chosen as pH is 3.
The catalyst of present embodiment uses the liquor zinci chloridi of highly acid, and it is molten can not only to neutralize the subsidiary alkalinity of raw material Liquid, while donor and acceptor center of the zinc chloride as electronics pair, can be with the 0H base of cellulose complex in wood material It has an effect, leads to the fracture of cellulosic molecule linkage, to play catalytic action.
A kind of optional embodiment as vacuum carburization processing.
The method that vacuum carburization is handled in the step S2 includes: step S21, and raw material is put into vacuum drying oven, and is taken out true Sky is to form vacuum environment;Step S22, heat drying;Step S23, microwave carbonization;And step S24, heating activation.
Optionally, the vacuum degree is typically maintained in 100Pa hereinafter, preferably 13Pa, 50 Pa.Vacuum pressure is lower, carbon The air changed in environment is fewer, and active carbon particle can be effectively prevented and adsorb carbon dioxide or dirt in air during the preparation process Angstrom impurity etc., guarantees its adsorbance to pigment in liquid glucose.
Optionally, the temperature of the heat drying is 250-300 DEG C, drying time 20-50min, to reduce in raw material Moisture.
Optionally, the power 400-550W of the microwave, radiated time 20-30min.
Optionally, the temperature of the heating activation is 850-1000 DEG C, activation time 100-150min.Ordinary circumstance Under, activation temperature is higher, and the activation duration is longer, and micropore of the pore radius less than 10 angstroms is easier by firing macropore, simultaneously.Cause This comprehensive energy consumption and adsorption effect, the temperature that heating activation can be set is 900 DEG C, activation time 120min.
The vacuum carburization processing of present embodiment regulates and controls it by the way that raw material is carbonized under vacuum conditions, is activated Microwave parameters (power, radiated time), activation parameter (activation temperature, activation time) etc., improve big in CharcoAid Hole ratio;The purity and adsorbance that can guarantee active carbon particle simultaneously, improve suction of the CharcoAid to pigment in liquid glucose Attached effect.
Embodiment 2
On the basis of embodiment 1, the present embodiment 2 provides a kind of CharcoAid, and the CharcoAid is suitable in vacuum Prepared under environment, with obtain high-purity, low impurity, high adsorption capacity active carbon particle.
Ingredient and specific implementation process about CharcoAid are discussed referring to the correlation of embodiment 1, and details are not described herein again.
In conclusion this CharcoAid and preparation method purify raw material by alkaline solution, catalyst is then carried out Catalysis, then under vacuum conditions carry out microwave carbonization, finally by washing and drying and etc. prepare craboraffin preparation, with Obtain high-purity, low impurity, high adsorption capacity active carbon particle;By in the liquor zinci chloridi of highly acid and the subsidiary alkali of raw material Property solution, and play catalytic action;By the way that carbonization-activation is handled under vacuum conditions by raw material, and regulate and control its microwave parameters, work Change parameter etc., improve the macropore ratio in CharcoAid, to improve the adsorption effect to pigment in liquid glucose.Therefore, this activity Charcoal preparation has many advantages, such as purity is high, macropore ratio height, large amount of adsorption, especially has significant absorption effect to the pigment in liquid glucose Fruit.
Embodiment 4
(1) pretreatment of raw material.After the raw material that 10kg partial size is 200 mesh is passed through sodium hydroxide solution, then it is impregnated in 40kg catalysis In agent;Wherein chlorination zinc concentration is 55wt%, pH value 2.5 in catalyst.
(2) carbonization treatment.First raw material is placed in the vacuum drying oven that vacuum degree is 100Pa, is heated to 250 DEG C of dryings 20min;Then pass through the microwave radiation 20min of 400W power;Finally it is warming up to 850 DEG C of activation 100min.
(3) it is rinsed with water, then dries, the CharcoAid is made.
Embodiment 5
(1) pretreatment of raw material.After the raw material that 10kg partial size is 300 mesh is passed through potassium hydroxide solution, then it is impregnated in 50kg catalysis In agent;Wherein chlorination zinc concentration is 60wt%, pH value 3 in catalyst.
(2) carbonization treatment.First raw material is placed in the vacuum drying oven that vacuum degree is 50Pa, is heated to 300 DEG C of dryings 50min;Then pass through the microwave radiation 30min of 550W power;Finally it is warming up to 950 DEG C of activation 100min.
(3) it is rinsed with water, then dries, the CharcoAid is made.
Embodiment 6
(1) pretreatment of raw material.After the raw material that 10kg partial size is 400 mesh is passed through calcium hydroxide solution, then it is impregnated in 70kg catalysis In agent;Wherein chlorination zinc concentration is 75wt%, pH value 4.5 in catalyst.
(2) carbonization treatment.First raw material is placed in the vacuum drying oven that vacuum degree is 13Pa, is heated to 280 DEG C of dryings 30min;Then pass through the microwave radiation 25min of 500W power;Finally it is warming up to 1000 DEG C of activation 150min.
(3) it is rinsed with water, then dries, the CharcoAid is made.
Embodiment 7
(1) pretreatment of raw material.After the raw material that 10kg partial size is 500 mesh is passed through sodium hydroxide solution, then it is impregnated in 60kg catalysis In agent;Wherein chlorination zinc concentration is 70wt%, pH value 3.5 in catalyst.
(2) carbonization treatment.First raw material is placed in the vacuum drying oven that vacuum degree is 75Pa, is heated to 300 DEG C of dryings 30min;Then pass through the microwave radiation 30min of 500W power;Finally it is warming up to 900 DEG C of activation 120min.
(3) it is rinsed with water, then dries, the CharcoAid is made.
Embodiment 8
(1) pretreatment of raw material.After the raw material that 10kg partial size is 300 mesh is passed through sodium hydroxide solution, then it is impregnated in 60kg catalysis In agent;Wherein chlorination zinc concentration is 65wt%, pH value 3.5 in catalyst.
(2) carbonization treatment.First raw material is placed in the vacuum drying oven that vacuum degree is 25Pa, is heated to 300 DEG C of dryings 30min;Then pass through the microwave radiation 30min of 450W power;Finally it is warming up to 880 DEG C of activation 120min.
(3) it is rinsed with water, then dries, the CharcoAid is made.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.

Claims (9)

1. a kind of preparation method of CharcoAid characterized by comprising
Pretreatment of raw material after raw material is passed through alkaline solution, then is impregnated in catalyst;
Vacuum carburization processing, i.e., carry out carbonization-activation for raw material under vacuum conditions;
Washing;And
Drying, is made the CharcoAid.
2. preparation method according to claim 1, which is characterized in that
The mass ratio of the raw material and catalyst is 1:4-7.
3. preparation method according to claim 1, which is characterized in that
The catalyst includes: zinc chloride, HCl and water;Wherein
Chlorination zinc concentration is 55-75wt%;
The pH value of catalyst is 2.5-4.5.
4. preparation method according to claim 1, which is characterized in that
The method of vacuum carburization processing includes:
Raw material is put into vacuum drying oven, and is vacuumized;
Heat drying;
Microwave carbonization;And
Heating activation.
5. the preparation method according to claim 4, which is characterized in that
The temperature of the heat drying is 250-300 DEG C, drying time 20-50min.
6. the preparation method according to claim 4, which is characterized in that
The power 400-550W of the microwave, radiated time 20-30min.
7. the preparation method according to claim 4, which is characterized in that
The temperature of the heating activation is 850-1000 DEG C, activation time 100-150min.
8. preparation method according to claim 1, which is characterized in that
The raw material is wooden clast, and partial size is 200-500 mesh.
9. a kind of CharcoAid, which is characterized in that
The CharcoAid is suitable for preparing under vacuum conditions.
CN201910466607.1A 2019-05-31 2019-05-31 Craboraffin preparation and preparation method thereof Pending CN110193346A (en)

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Application Number Priority Date Filing Date Title
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101544370A (en) * 2009-05-04 2009-09-30 成都信息工程学院 Method for producing active carbon by using traditional Chinese medicine dregs
US20110312485A1 (en) * 2010-06-18 2011-12-22 The Governors Of The University Of Alberta Method for preparation of activated carbon
CN102633259A (en) * 2012-03-26 2012-08-15 江苏紫荆花纺织科技股份有限公司 Preparation method for jute-based active carbon
CN103213986A (en) * 2013-05-03 2013-07-24 西北农林科技大学 Formula and preparation method of active carbon with ultra-high pore volume
CN103816868A (en) * 2014-03-03 2014-05-28 石河子大学 Mesoporous sugar beet pulp activated carbon and microwave-assisted preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101544370A (en) * 2009-05-04 2009-09-30 成都信息工程学院 Method for producing active carbon by using traditional Chinese medicine dregs
US20110312485A1 (en) * 2010-06-18 2011-12-22 The Governors Of The University Of Alberta Method for preparation of activated carbon
CN102633259A (en) * 2012-03-26 2012-08-15 江苏紫荆花纺织科技股份有限公司 Preparation method for jute-based active carbon
CN103213986A (en) * 2013-05-03 2013-07-24 西北农林科技大学 Formula and preparation method of active carbon with ultra-high pore volume
CN103816868A (en) * 2014-03-03 2014-05-28 石河子大学 Mesoporous sugar beet pulp activated carbon and microwave-assisted preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
薛智勇主编: "《农业固体废物处理与处置》", 30 November 2016, 河南科学技术出版社 *
韩笑 等: "木棉基活性炭纤维的制备及其对挥发性有机物的吸附性能", 《北京化工大学学报(自然科学版)》 *

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Application publication date: 20190903