CN110449129A - A kind of method and its application of soapberry residue preparation hydro-thermal charcoal - Google Patents
A kind of method and its application of soapberry residue preparation hydro-thermal charcoal Download PDFInfo
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- CN110449129A CN110449129A CN201910660263.8A CN201910660263A CN110449129A CN 110449129 A CN110449129 A CN 110449129A CN 201910660263 A CN201910660263 A CN 201910660263A CN 110449129 A CN110449129 A CN 110449129A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
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Abstract
The invention discloses a kind of method of soapberry residue preparation hydro-thermal charcoal, includes the following steps: that (1) is cleaned soapberry residue, after dry and crushing, obtain soapberry residue powder;(2) soapberry residue powder is mixed with water, and in 200~240 DEG C of 6~10h of charing, obtains carbonizing production, after cleaning by carbonizing production and is dry, obtain hydro-thermal charcoal;(3) after hydro-thermal charcoal being mixed with potassium hydroxide solution at 50~70 DEG C 0.5~2h of heating water bath, obtain heating water bath product, heating water bath product is uniformly mixed with melamine and ammonium hydroxide again, and 1~2h of back flow reaction at 55~65 DEG C, obtain back flow reaction product, after back flow reaction product is washed till neutrality and is dried, finished product is obtained.Preparation method of the invention solves soapberry residue and discards bring problem of environmental pollution, and recycling for waste resource may be implemented.The invention also discloses the applications of hydro-thermal charcoal pyridine in absorption coking wastewater.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of method of soapberry residue preparation hydro-thermal charcoal and its answer
With.
Background technique
All life activity originates from water, and water is the base substance to maintain biological life, protection and saving water resource
It is most important for us, and with the development of recent decades process of industrialization, the discharge amount of waste water increasingly increases, environmental pollution
Problem is severe and urgently to be resolved.Pyridine in waste water is colourless to be not easy to behave and discovers, and has toxicity, if it is not cleared to environment and
Human health has great harm.The comprehensive utilization of the biological materials such as agriculture and forestry organic waste material be always countries in the world environmental protection and
The important directions of Ecological Sustainable Development, and in recent years because of CO2、NO2And CH4The discharge amount increase of isothermal chamber gas causes
Climatic variation allows scientist to start to pay attention to the utilization of charcoal because it facilitates the mode sealed up for safekeeping by charcoal, capture with
The greenhouse gases in atmosphere are removed, highly stable form is converted them to, can be stored in the soil for thousands of years.But it passes
The biological carbon materials performance of system is unable to satisfy the requirement of high adsorption capacity in reality, needs the structure by further changing charcoal
To reach wider application.
Soapberry plants energetically in the whole nation especially Fujian Province as important energy kind tree, it is high to develop cultivated area
Up to 1.33 × 104km2.Soapberry is mainly used for extraction biodiesel raw material, and the residue after extraction is about 70% or so, nothing
Suffer from sub- residue and contain a large amount of cellulose, the content through the carbon in detection residue is up to 49.34%, and discarding both destroys ring
Border, and waste of resource.How effectively to take the measure of science to realize the resource utilization of soapberry residue, becomes soapberry
The problem that industry develops in a healthy way.
Therefore, a kind of method for preparing modified hydro-thermal charcoal using discarded soapberry residue is developed, it is discarded without trouble to realizing
Sub- residue high added value resource utilization has great importance.
Summary of the invention
It is an object of the invention to overcome above-mentioned technical deficiency, a kind of method for proposing soapberry residue preparation hydro-thermal charcoal,
The problem of discarded soapberry residue as resources of this method effective solution utilizes.The purpose of another aspect of the present invention is, mentions
A kind of application using hydro-thermal charcoal made from soapberry residue out.
To reach above-mentioned technical purpose, technical solution of the present invention provides a kind of side of soapberry residue preparation hydro-thermal charcoal
Method includes the following steps:
S1, soapberry residue is cleaned, after dry and crushing, obtains soapberry residue powder;
S2, the soapberry residue powder is mixed with water, and in 200~240 DEG C of 6~10h of charing, obtains charing and produce
Object after the carbonizing production is cleaned and dried, obtains hydro-thermal charcoal;
S3, the hydro-thermal charcoal is mixed with potassium hydroxide solution after at 50~70 DEG C 0.5~2h of heating water bath, obtain water
Heated Products are bathed, then the heating water bath product are uniformly mixed with the mixed liquor of melamine and ammonium hydroxide, and in 55~65 DEG C
1~2h of lower back flow reaction, obtains back flow reaction product, after the back flow reaction product is washed till neutrality and is dried, obtains finished product.
Technical solution of the present invention additionally provides a kind of pyrrole in absorption coking wastewater of hydro-thermal charcoal made from soapberry residue
The application of pyridine.
Compared with prior art, the beneficial effect comprise that
1, the present invention is raw material by carbonizing using soapberry residue, using potassium hydroxide solution, melamine and ammonium hydroxide
After activation, modified soapberry hydro-thermal charcoal is made, not only can solve soapberry residue and discarded bring problem of environmental pollution, but also can
To realize recycling for waste resource, maximally utilizing for waste resource is realized;
2, modified soapberry hydro-thermal carbon surface functional group's type produced by the present invention and hole are more, have higher
Specific surface area and good chemical stability, excellent absorption property, soapberry hydro-thermal charcoal obtained is to pyrrole in coking wastewater
Pyridine has preferable adsorption effect;
3, the present invention rationally utilizes agricultural wastes resource, really realizes that agricultural wastes are turned waste into wealth, is conducive to alleviate
The pressure of China's energy shortages, preserves the ecological environment, and promotes Ecological Civilization Construction, promotes the sustainable development of agricultural.
Detailed description of the invention
Fig. 1 is modification and unmodified soapberry hydro-thermal charcoal XRD diagram in the embodiment of the present invention 1;
Fig. 2 is the infrared spectrogram of the modification and unmodified soapberry hydro-thermal charcoal in the embodiment of the present invention 1;
Fig. 3 is that the SEM of the modification and unmodified soapberry hydro-thermal charcoal in the embodiment of the present invention 1 schemes, wherein (a) is not change
Property hydro-thermal charcoal, (b) be modified hydro-thermal charcoal;
Fig. 4 is influence of the throwing charcoal amount of modified hydro-thermal charcoal to adsorbance and adsorption rate;
Fig. 5 is the influence for being adsorbed the pH value of solution to the modified adsorbance and adsorption rate for throwing charcoal amount;
Fig. 6 is influence of the adsorption time to the modified adsorbance and adsorption rate for throwing charcoal amount.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that embodiment described herein is only used to explain the present invention, and do not have to
It is of the invention in limiting.
The embodiment provides a kind of methods of soapberry residue preparation hydro-thermal charcoal, include the following steps:
(1) soapberry residue is cleaned, after dry and crushing, obtains soapberry residue powder;
(2) soapberry residue powder is mixed with water, and in 200~240 DEG C of 6~10h of charing, obtains carbonizing production, it will
After carbonizing production cleaning and drying, hydro-thermal charcoal is obtained;
(3) after the hydro-thermal charcoal in step (2) being mixed with potassium hydroxide solution at 50~70 DEG C heating water bath 0.5~
2h obtains heating water bath product, then heating water bath product is uniformly mixed with the mixed liquor of melamine and ammonium hydroxide, and in 55~
1~2h of back flow reaction at 65 DEG C, obtains back flow reaction product, after back flow reaction product is washed till neutrality and is dried, obtains finished product.
Soapberry residue dries to 8 in some preferred embodiments of the invention, in step (1) at 100~110 DEG C~
12h, and soapberry residue is crushed to 80 mesh.
In some preferred embodiments of the invention, carbonization temperature is 220 DEG C in step (2), carbonization time 8h.
In some preferred embodiments of the invention, carbonizing production successively uses ethyl alcohol and deionized water clear in step (2)
It washes, filter, until filtrate is colourless and pH is 7, then dry at 100~110 DEG C to constant weight, obtain hydro-thermal charcoal.
In some preferred embodiments of the invention, the mass ratio of hydro-thermal charcoal and potassium hydroxide solution is in step (3)
1:2.5~3.5;It is highly preferred that the mass ratio of hydro-thermal charcoal and potassium hydroxide is 1:3.
In some preferred embodiments of the invention, the concentration of potassium hydroxide solution is 5mol/L.
In some preferred embodiments of the invention, water bath heating temperature is 60 DEG C in step (3), the heating water bath time
For 1h.
In some preferred embodiments of the invention, in step (3) in the mixed liquor of melamine and ammonium hydroxide, melamine
The molar ratio of amine and ammonium hydroxide is 18~22:1, and the concentration of ammonium hydroxide is 2mol/L;It is highly preferred that the molar ratio of melamine and ammonium hydroxide
For 20:1.
In some preferred embodiments of the invention, back flow reaction temperature is 60 DEG C in step (3), reflux time
For 1.5h.
The embodiments of the present invention also provide hydro-thermal charcoal made from a kind of soapberry residue absorption coking wastewater in pyridine
Application.
In some preferred embodiments of the invention, the pyrrole in absorption coking wastewater of hydro-thermal charcoal made from soapberry residue
When pyridine, the pH of coking wastewater is adjusted to 8~10, the dosage of hydro-thermal charcoal made from soapberry residue is 13.3g/L, adsorption time
For 2h.
In order to which the present invention will be described in further detail, the present invention is carried out below in conjunction with specific embodiment further
Explanation.Experimental method used in embodiment in the present invention is conventional method unless otherwise specified;Reality in the present invention
Material used in example, reagent etc. are applied, is that market is commercially available unless otherwise specified.
Embodiment 1:
The embodiment of the present invention 1 provides a kind of method of soapberry residue preparation hydro-thermal charcoal, includes the following steps:
(1) soapberry residue is cleaned, is dried at 105 DEG C, then crushed with high-speed multifunctional pulverizer, cross 80 mesh
Sieve, obtains soapberry residue powder;
(2) 25g soapberry residue powder is weighed, 100ml deionized water is added, stirring soaks soapberry residue powder sufficiently
Profit, is transferred in reaction kettle, the mixed liquor in reaction kettle is heated to 220 DEG C of charing 8h, then reaction kettle is naturally cooled to often
Temperature opens reaction kettle and pours out carbonizing production, cleaned respectively with ethyl alcohol and deionized water, filters carbonizing production, until filtrate is colourless
And pH is 7, dries at 105 DEG C to constant weight, obtains hydro-thermal charcoal;
It (3) is the water-bath 1h at 60 DEG C after 1:3 is mixed according to mass ratio with 5mol/L potassium hydroxide solution by hydro-thermal charcoal,
After being cleaned with deionized water, heating water bath product is obtained, then by the mixed liquor (three of heating water bath product and melamine and ammonium hydroxide
The molar ratio of poly cyanamid and ammonium hydroxide is 20:1) it is uniformly mixed, and the back flow reaction 1.5h at 60 DEG C, back flow reaction product is obtained,
Back flow reaction product is cleaned with deionized water to neutrality, dry 3~4h, obtains finished product at 105 DEG C.
Unmodified soapberry water obtained in the modified hydro-thermal charcoal of finished product soapberry obtained and step (2) in the present embodiment 1
The XRD diagram of hot charcoal is shown in Fig. 1.As seen from Figure 1, unmodified soapberry hydro-thermal charcoal is there are two apparent characteristic peak, 2 θ=
Diffraction maximum is more apparent between at 15 °~25 °, there is a gentle peak at 2 θ=34 °.The diffraction maximum of sample is relatively narrow and carries on the back relatively
Ground intensity is high, shows that its crystallinity is higher, and crystal grain is big, and crystal content is high.Modified hydro-thermal charcoal has diffraction at 2 θ=19 °~22 °
Peak, but diffraction maximum is wider, and intensity is also weaker.Show after potassium hydroxide, melamine and ammonium hydroxide activate, graphite-like structure is micro-
Crystal layer face can be destroyed, and pore structure can become larger.If hydro-thermal charcoal activation degree is further deepened, will appear microstructure without
Sequence, unformed phenomenon, already present pore structure aperture are further enlarged, and adsorption capacity can also enhance.If but activation degree
It is too deep, it will lead to hole " collapsing ", therefore to reasonably select activator species and concentration.
Unmodified soapberry water obtained in the modified hydro-thermal charcoal of finished product soapberry obtained and step (2) in the present embodiment 1
The infrared spectrogram of hot charcoal is shown in Fig. 2.Figure it is seen that hydro-thermal carbon surface has a functional group abundant, it is unmodified before
3409cm-1、2364cm-1、1403cm-1、1070cm-1Nearby there is peak value, is in 3409cm-1There is a wider absorption at place
Peak, 2364cm-1The absorption peak at place may be the stretching vibration area of triple carbon-carbon bonds and accumulative double bond, 1403cm-1Place may be alkene
C-H in-plane bending, 1070cm-1The generation of the absorption peak at place should be C-O stretching vibration.Modified hydro-thermal charcoal, in 3430cm-1The absorption peak at place weakens, may be with the hydroxyl in alcohol, phenol since modifying agent potassium hydroxide, melamine and ammonium hydroxide are in alkalinity
, newly there is 833cm in condensation dehydration-1Absorption peak out, shows to have that there are c h bonds and aromatic possibility.In general it is modified
Mainly there are phenol, alcoholic extract hydroxyl group, alkene, carbonyl etc. in hydro-thermal Tan Zhong functional group afterwards.
Unmodified soapberry water obtained in the modified hydro-thermal charcoal of finished product soapberry obtained and step (2) in the present embodiment 1
The SEM figure of hot charcoal is shown in Fig. 3, wherein (a) is unmodified hydro-thermal charcoal, (b) is modified hydro-thermal charcoal.As seen from Figure 3,
There are some bulks in figure (a) and without level column, hole is unobvious;And scheming surface in (b) has hole, structure is obvious, table
Face carbon block is more, and specific surface area is larger, therefore the adsorption effect of modified hydro-thermal charcoal is preferable.
Embodiment 2:
The embodiment of the present invention 2 provides a kind of method of soapberry residue preparation hydro-thermal charcoal, includes the following steps:
(1) soapberry residue is cleaned, is dried at 100 DEG C, then crushed with high-speed multifunctional pulverizer, cross 80 mesh
Sieve, obtains soapberry residue powder;
(2) 25g soapberry residue powder is weighed, 100ml deionized water is added, stirring soaks soapberry residue powder sufficiently
Profit, is transferred in reaction kettle, the mixed liquor in reaction kettle is heated to 200 DEG C of charing 10h, then reaction kettle is naturally cooled to often
Temperature opens reaction kettle and pours out carbonizing production, cleaned respectively with ethyl alcohol and deionized water, filters carbonizing production, until filtrate is colourless
And pH is 7, dries at 110 DEG C to constant weight, obtains hydro-thermal charcoal;
It (3) is the water-bath at 70 DEG C after 1:3.5 is mixed according to mass ratio with 5mol/L potassium hydroxide solution by hydro-thermal charcoal
0.5h after being cleaned with deionized water, obtains heating water bath product, then by the mixing of heating water bath product and melamine and ammonium hydroxide
Liquid (molar ratio of melamine and ammonium hydroxide is 22:1) is uniformly mixed, and the back flow reaction 2h at 65 DEG C, obtains back flow reaction production
Object cleans back flow reaction product to neutrality with deionized water, and dry 3~4h, obtains finished product at 105 DEG C.
Embodiment 3:
The embodiment of the present invention 3 provides a kind of method of soapberry residue preparation hydro-thermal charcoal, includes the following steps:
(1) soapberry residue is cleaned, is dried at 110 DEG C, then crushed with high-speed multifunctional pulverizer, cross 80 mesh
Sieve, obtains soapberry residue powder;
(2) 25g soapberry residue powder is weighed, 100ml deionized water is added, stirring soaks soapberry residue powder sufficiently
Profit, is transferred in reaction kettle, the mixed liquor in reaction kettle is heated to 240 DEG C of charing 6h, then reaction kettle is naturally cooled to often
Temperature opens reaction kettle and pours out carbonizing production, cleaned respectively with ethyl alcohol and deionized water, filters carbonizing production, until filtrate is colourless
And pH is 7, dries at 100 DEG C to constant weight, obtains hydro-thermal charcoal;
It (3) is the water-bath at 50 DEG C after 1:2.5 is mixed according to mass ratio with 5mol/L potassium hydroxide solution by hydro-thermal charcoal
2h after being cleaned with deionized water, obtains heating water bath product, then by the mixed liquor of heating water bath product and melamine and ammonium hydroxide
(molar ratio of melamine and ammonium hydroxide is 18:1) is uniformly mixed, and the back flow reaction 1h at 55 DEG C, obtains back flow reaction product,
Back flow reaction product is cleaned with deionized water to neutrality, dry 3~4h, obtains finished product at 105 DEG C.
Embodiment 4:
When the present embodiment has inquired into pyridine in hydro-thermal charcoal absorption waste water, the optimal addn of hydro-thermal charcoal is specific using as follows
Method: weighing modified hydro-thermal charcoal obtained in embodiment 1, using initially throw charcoal amount as variable (throw charcoal amount be respectively 0.05g, 0.1g,
0.2g, 0.3g, 0.4g, 0.5g), it keeps other consistent, i.e., at normal temperature, shakes in case and adsorbed with the revolving speed of 150r/min
Volume is 30mL, and concentration is the pyridine solution of 0.03ml/L, and the pH of every part of pyridine solution is identical, adsorbs 4h.After take
Clear liquid, measures the absorbance (wavelength 257nm, using distilled water as reference) of every part of solution with ultraviolet specrophotometer, and with mark
The concentration of directrix curve equation calculation residue pyridine calculates adsorbance and adsorption rate, obtains Fig. 4.
As seen from Figure 4, when throwing charcoal amount is greater than 0.4g, i.e., when the throwing charcoal amount of modified hydro-thermal charcoal is greater than 13.3g/L, water
Hot charcoal is larger to the adsorbance of pyridine, illustrates that the dosage for increasing hydro-thermal charcoal can increase active adsorption sites, promotes adsorption capacity,
But the amount of hydro-thermal charcoal is too many, and not only resulting in the wasting of resources also will increase processing cost, therefore, the best throwing charcoal of modified hydro-thermal charcoal
Amount is 13.3g/L.
Embodiment 5:
When the present embodiment has inquired into pyridine in hydro-thermal charcoal absorption waste water, it is adsorbed the Optimal pH of solution, it is specific using as follows
Method: weighing modified hydro-thermal charcoal obtained in embodiment 1, using pH as variable (pH is respectively 2,4,6,7,8,10), keeps other
It is consistent, i.e., at normal temperature, hydro-thermal charcoal 0.1g is put into concussion case, is 30mL with the revolving speed adsorption volume of 150r/min,
Concentration is the pyridine solution of 0.03ml/L, adsorbs 4h.After take supernatant, measure every part of solution with ultraviolet specrophotometer
Absorbance (wavelength 257nm, using distilled water as reference), and the concentration of remaining pyridine is calculated with calibration curve equation, it calculates and inhales
Attached amount and adsorption rate, obtain Fig. 5.
As seen from Figure 5, adsorbance increases with the increase of pH, but when pH it is excessively high, alkaline solution and pyrrole can be enhanced
Affinity between pyridine, therefore, the Optimal pH of modified hydro-thermal charcoal Adsorption of Pyridine are 8~10.
Embodiment 6:
The present embodiment has inquired into optimal adsorption time when pyridine in hydro-thermal charcoal absorption waste water, specifically with the following method:
Weigh modified hydro-thermal charcoal obtained in embodiment 1, using adsorption time as variable (adsorption time be respectively 20min, 40min,
60min, 120min, 180min, 240min), it keeps other conditions consistent, i.e., at normal temperature, puts into hydro-thermal charcoal into concussion case
0.1g, the revolving speed adsorption volume with 150r/min are 30mL, and concentration is the pyridine solution of 0.03ml/L, and every part of pyridine solution
PH is identical.After take supernatant liquor, measure absorbance with ultraviolet specrophotometer, calculate remaining pyridine concentration, calculate absorption
Amount and adsorption rate, obtain Fig. 6.
As seen from Figure 6, with the increase of adsorption time, adsorbance increases, and when adsorption time is greater than 120min, inhales
Attached amount is basically unchanged, and therefore, the optimal adsorption time of modified hydro-thermal charcoal is 120min.
Comparative example 1:
This example has been inquired into using different solution modification hydro-thermal charcoals, adsorbance and suction of the obtained modification hydro-thermal charcoal to pyridine
Attached rate.Hydro-thermal charcoal obtained is as hydro-thermal charcoal 1 using in embodiment 1;Hydro-thermal charcoal 2, area are prepared using method same as Example 1
It is not, 2moL/L sodium hydroxide solution is used in step (3);Hydro-thermal charcoal 3, area are prepared using method same as Example 1
It is not, 4moL/L sodium chloride solution is used in step (3);Hydro-thermal charcoal 4, difference are prepared using method same as Example 1
Be, use in step (3) mass fraction for 20% phosphoric acid solution.Again respectively by embodiment 1 in step (2) it is obtained not
Modified hydro-thermal charcoal, hydro-thermal charcoal 1, hydro-thermal charcoal 2, hydro-thermal charcoal 3 and hydro-thermal charcoal 4 is separately added into concussion case, and throwing charcoal amount is 0.1g, In
Under room temperature, the revolving speed adsorption volume with 150r/min is 30mL, and concentration is the pyridine solution of 0.03ml/L, and every part of pyridine solution
PH it is identical, adsorb 4h.Obtain result as shown in Table 1.
The absorption property result of the different modified hydro-thermal charcoals of table 1
As can be seen from Table 1, unmodified hydro-thermal charcoal is placed in different activators after activating, with unmodified hydro-thermal
Charcoal is compared, and the adsorption effect of the hydro-thermal charcoal after activation increases, wherein the hydro-thermal charcoal after being activated using potassium hydroxide solution
Adsorbance and adsorption effect it is best.Thus it can also be seen that soapberry residue hydro-thermal can be effectively improved after the activation of hydro-thermal charcoal
The absorption property of charcoal substantially increases the application prospect of soapberry hydro-thermal charcoal.
The above described specific embodiments of the present invention are not intended to limit the scope of the present invention..Any basis
Any other various changes and modifications that technical concept of the invention is made should be included in the guarantor of the claims in the present invention
It protects in range.
Claims (10)
1. a kind of method of soapberry residue preparation hydro-thermal charcoal, which comprises the steps of:
S1, soapberry residue is cleaned, after dry and crushing, obtains soapberry residue powder;
S2, the soapberry residue powder is mixed with water, and in 200~240 DEG C of 6~10h of charing, obtains carbonizing production, it will
After the carbonizing production cleaning and drying, hydro-thermal charcoal is obtained;
S3, the hydro-thermal charcoal is mixed with potassium hydroxide solution after at 50~70 DEG C 0.5~2h of heating water bath, obtain water-bath and add
Hot, then the heating water bath product is uniformly mixed with the mixed liquor of melamine and ammonium hydroxide, and next time in 55~65 DEG C
Stream 1~2h of reaction, obtains back flow reaction product, after the back flow reaction product is washed till neutrality and is dried, obtains finished product.
2. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that will in the step S1
Soapberry residue dries 8~12h at 100~110 DEG C, and soapberry residue is crushed to 80 mesh.
3. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that charcoal in the step S2
Changing temperature is 220 DEG C, carbonization time 8h.
4. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that charcoal in the step S2
Change product successively to be cleaned, filtered with ethyl alcohol and deionized water, until filtrate is colourless and pH is 7, then the drying at 100~110 DEG C
To constant weight, hydro-thermal charcoal is obtained.
5. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that water in the step S3
The mass ratio of hot charcoal and potassium hydroxide solution is 1:2.5~3.5.
6. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that hydrogen in the step S3
The concentration of potassium oxide solution is 5mol/L.
7. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that water in the step S3
Bathing heating temperature is 60 DEG C, and the heating water bath time is 1h;Back flow reaction temperature is 60 DEG C, reflux time 1.5h.
8. the method for soapberry residue preparation hydro-thermal charcoal according to claim 1, which is characterized in that institute in the step S3
In the mixed liquor for stating melamine and ammonium hydroxide, the molar ratio of melamine and ammonium hydroxide is 18~22:1, and the concentration of ammonium hydroxide is 2mol/
L。
9. a kind of pyrrole in absorption coking wastewater of hydro-thermal charcoal made from soapberry residue as described in any one of claims 1 to 8
The application of pyridine.
10. the application of the pyridine in absorption coking wastewater of hydro-thermal charcoal made from soapberry residue according to claim 9,
It is characterized in that, the pH of coking wastewater is 8~10, and the dosage of hydro-thermal charcoal made from soapberry residue is 13.3g/L, adsorption time
For 2h.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104069814A (en) * | 2014-07-11 | 2014-10-01 | 南开大学 | Method for preparing modified wood chip hydrothermal charcoal by adopting KOH |
CN104140101A (en) * | 2014-08-18 | 2014-11-12 | 福建师范大学 | Method for preparing activated carbon with ultrahigh specific surface area from soapberry residue as raw material |
CN107651687A (en) * | 2017-11-16 | 2018-02-02 | 湘潭大学 | A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen |
CN109529783A (en) * | 2019-01-08 | 2019-03-29 | 滨州学院 | Amino modified charcoal preparation method |
-
2019
- 2019-07-22 CN CN201910660263.8A patent/CN110449129A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104069814A (en) * | 2014-07-11 | 2014-10-01 | 南开大学 | Method for preparing modified wood chip hydrothermal charcoal by adopting KOH |
CN104140101A (en) * | 2014-08-18 | 2014-11-12 | 福建师范大学 | Method for preparing activated carbon with ultrahigh specific surface area from soapberry residue as raw material |
CN107651687A (en) * | 2017-11-16 | 2018-02-02 | 湘潭大学 | A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen |
CN109529783A (en) * | 2019-01-08 | 2019-03-29 | 滨州学院 | Amino modified charcoal preparation method |
Non-Patent Citations (2)
Title |
---|
YU WANG, ET AL.: "Amino-functionalized biomass-derived porous carbons with enhanced aqueous adsorption affinity and sensitivity of sulfonamide antibiotics", 《BIORESOURCE TECHNOLOGY》 * |
徐汉江: "芒果树皮生物炭的制备及其对吡啶和喹啉的吸附性能研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113117644A (en) * | 2021-03-24 | 2021-07-16 | 长江大学 | Preparation method and application of modified toona sinensis seed hydrothermal carbon |
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