CN105197926A - Method for preparing activated carbon with enzymatic hydrolysis lignin as raw material - Google Patents
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Abstract
The invention discloses a method for preparing activated carbon with enzymatic hydrolysis lignin as the raw material. The method comprises the following steps that the enzymatic hydrolysis lignin is mixed with one or more kinds of inorganic salt including chloride, sulfate, nitrate and the like according to the mass ratio of 1:(1-5); treatment is conducted for 0.5-2 h at the temperature of 50-180 DEG C in a kneading, squeezing and other modes; the obtained mixed materials are heated to 400-900 DEG C at the temperature raising speed of 1-5 DEG C/min and then subjected to heat treatment carbonization for 1-2 h; carbonized materials are taken out after cooling is achieved and washed with diluted hydrochloric acid or deionized water, the inorganic salt is recycled and washed with deionized water until the pH of filter liquor is 6-7, drying to the constant weight is conducted at 100-150 DEG C, and the activated carbon product is obtained. By means of the method, the activated carbon product which is high in specific surface area and iodine sorption value and is well developed in pore structure is prepared, and a new application approach is provided for comprehensively using lignin waste residues in the chemical processing process of plant fiber raw materials.
Description
Technical field
The invention belongs to chemical production technical field, being specifically related to a kind of take enzymolysis xylogen as the method that gac prepared by raw material.
Background technology
Plant fiber material is biomass material, is the main species that biomass processing utilizes.It is Mierocrystalline cellulose, hemicellulose and xylogen that the primary chemical of plant fiber material is formed, and wherein Mierocrystalline cellulose and hemicellulose are high glycan, are aliphatic carbon chain macromolecular compounds; Xylogen is the cross-linked type macromolecule that a class contains aromatic ring, has tridimensional network.In the chiral process of plant fiber material, high glycan, due to reasons such as chemical structure relatively simply, are easily degraded, therefore, is easily utilized by degraded, and xylogen is due to reasons such as complex structures, and processing and utilization is more difficult.The difficult problem that the raw material availability that these characteristics cause plant fiber material chemical process to utilize is low.Utilize in process in biomass chemical process, xylogen often becomes the waste residue that processing and utilization process produces, and not only greatly have impact on the utilising efficiency of raw material, and causes environmental pollution.Such as, in slurrying field, xylogen is exactly the main source that pulp industry causes severe contamination, is also the key issue that the comprehensive utilization of this field needs to solve.Therefore, the xylogen waste residue further modification processing and utilization that plant fiber material processing and utilization process produces is changed into all kinds of chemical or material, is the necessary ways of people's efficiency utilization plant fiber material.It is the material such as chemical containing aromatic ring and polymer, Carbon fibe and gac that existing much research reports lignin conversion.
At present, plant fiber material by after acid hydrolysis and enzymic hydrolysis, by Mierocrystalline cellulose and hemicellulose degradation, obtain monose and oligose, and be dissolved in water solvent, by further chemistry and biological chemistry processing, fuels and chemicals can be converted into, remaining residue then mainly xylogen.Therefore, utilize in process in biomass processing, the acid-hydrolysis lignin produced and enzymolysis xylogen are the main lignin residue kinds of two classes.The utilization of traditional acid-hydrolysis lignin has the research and development history of decades, such as, acid-hydrolysis lignin is converted into the products such as phenolic compound, phenolic aldehyde sizing agent and gac.And enzymolysis xylogen produces in the modern biochemistry processing and utilization process of plant fiber material, its utilization also just starts.
Because acid hydrolysis conditions is violent, and there is remarkable change in the molecular structure of xylogen in acid condition, and some xylogen can be dissolved in acid solution, and significant polymerization then occurs some xylogen; And enzymolysis xylogen carries out under mild hydrolysis condition, the change of lignin structure is different from acid hydrolysis conditions.And for plant fiber material, acid hydrolysis causes vegetable cell wall construction to be totally disrupted, enzymic hydrolysis then part remains vegetable cell wall construction.Because they must cause the processing and utilization Method and Process of acid hydrolysis and enzymic hydrolysis xylogen to have very big-difference in chemical constitution and structural significant difference.
Gac is the carbon absorbent that a class pore texture is flourishing, specific surface area is high, has been widely used in the various fields such as environment protection, chemical industry, foodstuffs industry, hydrometallurgy, medicine are refining, military chemistry protection.Produce the raw material mainly plant fiber material such as coal and timber, bamboo wood, shell of gac, the main method adopted is gas activation (also referred to as physical activation method) and pharmaceutical chemicals activation method.
Now there are some researches show, adopt the vegetable fibres such as pharmaceutical chemicals Activation of Wood, main material and stalk to prepare the precondition of gac and key factor is that pharmaceutical chemicals will permeate and be distributed to raw material inside.But, due to the firm cell wall structure that these raw materials have, under normal circumstances, the solution that pharmaceutical chemicals is prepared is difficult to penetrate into cell walls inside, better can not be distributed in the material network of Mierocrystalline cellulose, hemicellulose and xylogen formation, so after carbonizing and wash out chemical reagent, flourishing pore texture can not be formed, namely can not reach good activation effect, the quality of gac is just very poor.The present inventor prepared in the research and development work of gac at employing phosphoric acid activation plant fiber material in the past, delivered and applied for paper and Patents (Carbon, 2009,47 (15): 3578-3580; And be applied to production practice ZL200910184645.4).In actual industrial production process, the Mierocrystalline cellulose had due to zinc chloride and phosphoric acid moistens rise effect and acid hydrolysis effect, therefore better can penetrate into these plant cell wall inside configuration, thus produce the activated carbon product of hole prosperity.But other inorganics, as magnesium chloride, sodium-chlor all do not have effect.Another kind of situation is that soluble carbon containing low molecular weight organic compound can well mix in water or other solvent with inorganic chemical reagent, even Homogeneous phase mixing, is very beneficial in theory preparing pore texture prosperity and regulation and control pore texture.But the acute variation such as due in carbonization process, so organic and inorganic mixture can melt, contraction, cause the pore texture also not too prosperity formed, pore texture regulation and control become very complicated.Therefore, all user demand can't be met completely.
In pharmaceutical chemicals reactivation process, activator easily volatilized and the problem such as comparatively Heavy environmental pollution produced in the past.Industrial used pharmaceutical chemicals activation method was zinc chloride activation method and phosphoric acid activation method in the past.Wherein zinc chloride is 400
oa large amount of volatilization after more than C, and zinc chloride activation needs 550 usually
omore than C, so zinc chloride activation method can produce serious environmental pollution, to such an extent as to China has prohibitted the use the zinc chloride activation of flattening oven to produce the technological line of gac.Compared with zinc chloride activation method, phosphoric acid activation method due to the volatility of phosphoric acid relatively low, its pollution produced is much lower, but due to phosphoric acid be a kind of stronger acid, is combined with other composition of raw material the volatile matter generating other, and easy etching apparatus.Also be in the chemical activation method of KOH and NaOH of development phase, then due to needs 800
othe high temperature of more than C, and the metal simple-substance very easily producing blast can be discharged in reactivation process, cause great safety obstacle to scale operation.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of this invention is to provide a kind of take enzymolysis xylogen as the method that gac prepared by raw material, avoids activator in reactivation process easily to volatilize and the comparatively Heavy environmental pollution problem produced.
Technical scheme: for achieving the above object, the technical solution used in the present invention is as follows:
Take enzymolysis xylogen as the method that gac prepared by raw material, comprise the steps:
(1) enzymolysis xylogen, inorganic salt are mixed according to the mass ratio of 1:1 ~ 5, at 50 ~ 180 DEG C adopt knead, fashion of extrusion process 0.5 ~ 2h; Wherein enzymolysis xylogen is solid, and inorganics is the aqueous solution;
(2) after the material after process being warming up to 400 ~ 900 DEG C with the temperature rise rate of 1 ~ 5 DEG C/min, heat treatment carbonization 1 ~ 2h;
(3) take out carbonized material, with deionized water or dilute hydrochloric acid washing carbonized material, remove inorganic salt, finally make the pH of filtrate be 6 ~ 7, at 100 ~ 150 DEG C, be dried to weight, obtain activated carbon product.
In step (1), described enzymolysis xylogen is the solid residues of plant fiber material after biological enzyme hydrolysis such as timber, bamboo wood and stalk.
In step (1), described inorganics is the muriate such as zinc chloride, magnesium chloride, iron(ic) chloride, sodium-chlor, calcium chloride that can be water-soluble, the vitriol such as sodium sulfate, potassium sulfate, one or more in the inorganic salt such as nitrate such as magnesium nitrate, nitrocalcite, saltpetre.
In step (1), kneading with the temperature of extruding is 50-170 DEG C.
In step (2), carbonization temperature is 400-900 DEG C.
Beneficial effect: of the present invention take enzymolysis xylogen as the method that gac prepared by raw material, successfully adopts different types of inorganic salt as activator is that raw material has been prepared specific surface and reached 1000m with enzymolysis xylogen
2about/g, iodine sorption value can reach the more flourishing activated carbon product of the pore texture of 1200mg/g.In this inventive method, adopt the inorganic salt such as sodium-chlor, magnesium chloride and the calcium chloride that volatility is very low as activator, can greatly to avoid in reactivation process in the past in pharmaceutical chemicals reactivation process activator easily volatilize and the comparatively Heavy environmental pollution problem produced, visible, the gac that the present invention adopts chemistry for activation enzymolysis xylogen to prepare pore texture prosperity is a method having very much application prospect, is also that the waste material produced in comprehensive utilization plant fiber material chiral process provides an extraordinary application approach.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material proportion, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1
Calcium chloride being mixed with mass percent is 50%, take 10 grams of dry enzymolysis straw lignins, the ratio being 1:1 according to enzymolysis xylogen and the mass ratio of calcium chloride mixes, at 80 DEG C, extrude 1h, but in tube furnace, to be warming up to 700 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, takes out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7,120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1070m
2/ g, total pore volume is 0.684cm
3/ g.The iodine sorption value of gac is 890mg/g, and Methylene blue adsorption is 70mL/g.
Embodiment 2
Calcium chloride being mixed with mass percent is 70%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of calcium chloride mixes, at 80 DEG C, extrude 1h, but in tube furnace, to be warming up to 700 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, takes out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7,120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1430m
2/ g, total pore volume is 0.935cm
3/ g.The iodine sorption value of gac is 1271mg/g, and Methylene blue adsorption is 100mL/g.
Embodiment 3
Calcium chloride and sodium-chlor are mixed according to the mass ratio of 1:1, and be mixed with the solution that mass percent is 50%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of inorganic salt mixt calcium chloride mixes, 1h is extruded at 80 DEG C, but in tube furnace, to be warming up to 700 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, take out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7, 120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 981m
2/ g, total pore volume is 0.594cm
3/ g.The iodine sorption value of gac is 824mg/g, and Methylene blue adsorption is 50mL/g.
Embodiment 4
Sodium-chlor being mixed with mass percent is 70%, takes the enzymolysis straw lignin of 10g drying, and the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of calcium chloride mixes, at 80 DEG C, extrude 2h, but in tube furnace, with 5
obe warming up to 800 DEG C under the temperature rise rate of C/min, activation 1h, be cooled to taking-ups after 200 DEG C below, be washed till till filtrate pH reaches 6-7 with deionized water, 120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 998m
2/ g, total pore volume is 0.540cm
3/ g.The iodine sorption value of gac is 826mg/g, and Methylene blue adsorption is 50mL/g.
Embodiment 5
Calcium chloride and magnesium chloride are mixed according to the mass ratio of 1:1, and be mixed with the solution that mass percent is 50%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of inorganic salt mixt calcium chloride mixes, 1h is extruded at 100 DEG C, but in tube furnace, to be warming up to 700 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, take out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7, 120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1354m
2/ g, total pore volume is 0.798cm
3/ g.The iodine sorption value of gac is 1100mg/g, and Methylene blue adsorption is 110mL/g.
Embodiment 6
Calcium chloride and zinc chloride are mixed according to the mass ratio of 2:1, and be mixed with the solution that mass percent is 70%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of inorganic salt mixt calcium chloride mixes, 1h is extruded at 100 DEG C, but in tube furnace, to be warming up to 600 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, take out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7, 120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1289m
2/ g, total pore volume is 1.023cm
3/ g.The iodine sorption value of gac is 1020mg/g, and Methylene blue adsorption is 150mL/g.
Embodiment 7
Potassium sulfate being mixed with mass percent is 50%, takes the enzymolysis straw lignin of 10g drying, and the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of potassium sulfate mixes, at 100 DEG C, extrude 2h, but in tube furnace, with 5
obe warming up to 600 DEG C under the temperature rise rate of C/min, activation 1h, be cooled to taking-ups after 200 DEG C below, be washed till till filtrate pH reaches 6-7 with deionized water, 120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1083m
2/ g, total pore volume is 0.781cm
3/ g.The iodine sorption value of gac is 937mg/g, and Methylene blue adsorption is 60mL/g.
Embodiment 8
Magnesium nitrate is mixed with the aqueous solution that mass percent is 50%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of magnesium nitrate mixes, 2h is extruded at 70 DEG C, but in tube furnace, to be warming up to 650 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, take out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7,120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 785m
2/ g, total pore volume is 0.754cm
3/ g.The iodine sorption value of gac is 720mg/g, and Methylene blue adsorption is 120mL/g.
Embodiment 9
Calcium chloride being mixed with mass percent is 70%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:2 according to enzymolysis xylogen and the mass ratio of calcium chloride mixes, and knead extruding 2h at 140 DEG C, but in tube furnace, to be warming up to 800 DEG C under the temperature rise rate of 5 DEG C/min, activation 1h, takes out after being cooled to less than 200 DEG C, carbonized material is washed with dilute hydrochloric acid, reclaim inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7,120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1210m
2/ g, total pore volume is 0.826cm
3/ g.The iodine sorption value of gac is 1189mg/g, and Methylene blue adsorption is 80mL/g.
Embodiment 10
Magnesium chloride being mixed with mass percent is 70%, take the enzymolysis straw lignin of 10g drying, the ratio being 1:3 according to enzymolysis xylogen and the mass ratio of magnesium chloride mixes, knead extruding 2h at 110 DEG C, then dry moisture of going out in material at 120 DEG C, dried material is put into tube furnace, with 5
obe warming up to 700 DEG C under the temperature rise rate of C/min, activation 1h, be cooled to after 200 DEG C below and take out, wash carbonized material with dilute hydrochloric acid, recovery inorganic salt, finally with deionized water wash material to filtrate pH reaches 6-7,120 DEG C of dryings obtain Product Activity charcoal.Its specific surface area is 1480m
2/ g, total pore volume is 1.26cm
3/ g.The iodine sorption value of gac is 1330mg/g, and Methylene blue adsorption is 180mL/g.
Claims (6)
1. be the method that gac prepared by raw material with enzymolysis xylogen, it is characterized in that, comprise the steps:
(1) enzymolysis xylogen is mixed with the mass ratio of inorganic salt according to 1:1 ~ 5, at 50 ~ 180 DEG C adopt knead, fashion of extrusion process 0.5 ~ 2h; Wherein enzymolysis xylogen is solid, and inorganic salt are the aqueous solution;
(2) after the material after process being warming up to 400 ~ 900 DEG C with the temperature rise rate of 1 ~ 5 DEG C/min, heat treatment carbonization 1 ~ 2h;
(3) take out carbonized material, with dilute hydrochloric acid or deionized water wash carbonized material, reclaim inorganic salt, and be till 6 ~ 7 with the pH that deionized water is washed till filtrate, at 100 ~ 150 DEG C, be dried to weight, obtain activated carbon product.
2. according to claim 1 take enzymolysis xylogen as the method that gac prepared by raw material, it is characterized in that, in step (1), described enzymolysis xylogen raw material is the solid residues of plant fiber material after biological enzyme hydrolysis such as timber, bamboo wood and stalk, and its main ingredient is xylogen.
3. according to claim 1 is the method that gac prepared by raw material with enzymolysis xylogen, it is characterized in that, in step (1), described inorganic salt are muriate that can be water-soluble, vitriol, one or more in nitrate.
4. according to claim 3 is the method that gac prepared by raw material with enzymolysis xylogen, it is characterized in that, in step (1), described muriate is zinc chloride, magnesium chloride, iron(ic) chloride, sodium-chlor, calcium chloride; Vitriol is sodium sulfate, potassium sulfate; Nitrate is magnesium nitrate, nitrocalcite, saltpetre.
5. according to claim 1 is the method that gac prepared by raw material with enzymolysis xylogen, it is characterized in that, in step (1), kneading with the temperature of extruding is 50-170 DEG C.
6. according to claim 1 is the method that gac prepared by raw material with enzymolysis xylogen, it is characterized in that, in step (2), carbonization temperature is 400-900 DEG C.
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| CN107304048A (en) * | 2016-04-12 | 2017-10-31 | 东北林业大学 | A kind of preparation method of polyacrylic acid grafted lignin porous charcoal |
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| CN107254791B (en) * | 2017-06-07 | 2019-05-14 | 潞城市创蓝生物科技有限公司 | A kind of method of waste crop straws resource utilization |
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| CN113880091A (en) * | 2021-11-10 | 2022-01-04 | 天津科技大学 | Method for preparing magnetic activated carbon by treating papermaking black liquor with composite metal salt |
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Application publication date: 20151230 |