CN106994331A - The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material - Google Patents
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material Download PDFInfo
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- CN106994331A CN106994331A CN201710272297.0A CN201710272297A CN106994331A CN 106994331 A CN106994331 A CN 106994331A CN 201710272297 A CN201710272297 A CN 201710272297A CN 106994331 A CN106994331 A CN 106994331A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid 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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- Treatment Of Sludge (AREA)
Abstract
The invention discloses a kind of method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, belong to sewage treatment area.This method comprises the following steps：（1）It is 4~7% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains mud granule；（2）Activator, Phenoxyethanol, hydroxymethyl cellulose and sodium chloride are added to the water, mud granule is added after dissolving, is soaked, is dried；（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, heating, charing pyrolysis；（4）Hydrochloric acid solution containing product is heated in water-bath, neutrality is washed to, grinding is dry, pulverize, 200 mesh sieves is crossed, obtains shale charcoal sorbing material.Mud granule is carried out after immersion treatment using the method for the present invention, the adsorption capacity of the output of final shale charcoal, Phenoxyethanol and zinc oxide collaboration enhancing shale charcoal can be improved.
Description
Technical field
The present invention discloses one kind and belongs to sewage treatment area, more particularly to a kind of paper-making industrial waste water sludge prepares shale charcoal
The method of sorbing material.
Background technology
Paper-making industrial waste water sludge is usually the volatilization in fiber, hydrophilic metal hydroxide, biological treatment structures
Property material.
Application No. CN201310565263.2 Chinese patent application discloses a kind of wastewater sludge processing method, we
Method is that first wastewater sludge is dehydrated to the pretreating sludge that moisture content is 88%~90%, adds iron chloride and is well mixed, then
The pH value of the pretreating sludge is adjusted using aqua calcis, flyash is added and is well mixed, finally using filter press
It is pressed into the clod of moisture content≤50%.Compared with prior art, the invention enters in terms of broken wall modification and mechanism filter-pressing matching
Hand, by sludge dewatering to moisture content below 50%, and dehydration after sludge there is hydrophobicity, secondary sludge will not be produced.But
Subsequent treatment for sludge still wastes sizable resource.
The content of the invention
There is provided a kind of paper-making industrial waste water sludge system for the problem of present invention is in order to solve prior art paper-making industrial waste water
The method of standby shale charcoal sorbing material, by being recycled to sludge, adsorption material is obtained while realizing water reuse
Material, the not only environmentally friendly but also saving energy.
In order to solve the above-mentioned technical problem, the present invention uses following technical scheme：
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 4~7% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Particle；
（2）By weight, by 1~2 part of activator, 6~10 parts of Phenoxyethanols, 4~10 parts of hydroxymethyl celluloses and 2~5 parts
Sodium chloride is added in 20~30 parts of water, and 1~2 part of mud granule is added after dissolving, is soaked 1-3 hours, soaking temperature is 30-50
DEG C, dry；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 800~850 DEG C are warming up to,
15~90min of charing pyrolysis；
（4）By the hydrochloric acid solution containing product in 60~80 DEG C of water-baths 1~3min of heating response, be washed to neutrality, dry, powder
Breakdown mill, crosses 200 mesh sieves, obtains shale charcoal sorbing material.
Preferably, step（1）Moisture content be 5%.
Preferably, step（2）In each raw material include：1.2 parts of activators, 8 parts of Phenoxyethanols, 6 parts of hydroxymethyl celluloses,
3 parts of sodium chloride, 27 parts of water and 1.2 parts of mud granules.
Preferably, described activator is the zinc chloride that mass concentration is 1~5mol/L.
Preferably, step（3）Reaction temperature be 830 DEG C, the reaction time is 50min.
Preferably, step（4）The concentration 2mol/L of middle hydrochloric acid solution.
The invention has the advantages that：The shale charcoal yield of the present invention is 76~78%, and iodine sorption value is up to 640mg/
G, is illustrated to carry out after immersion treatment mud granule using the method for the present invention, can improve the output of final shale charcoal, benzene
The adsorption capacity of oxyethanol and zinc oxide collaboration enhancing shale charcoal.
Embodiment
The present invention is further described in detail with reference to specific embodiment.
Embodiment 1
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 5% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Grain；
（2）By weight, by zinc chloride, 8 part Phenoxyethanol, 6 part hydroxymethyl celluloses of 1.2 parts of mass concentrations for 3mol/L
Added with 3 parts of sodium chloride in 27 parts of water, 1.2 parts of mud granules are added after dissolving, soaked 2 hours, soaking temperature is 40 DEG C, is done
It is dry；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 830 DEG C, charing heat are warming up to
Solve 50min；
（4）By the hydrochloric acid solution of the concentration 2mol/L containing product in 70 DEG C of water-baths heating response 2min, be washed to neutrality, do
Dry, attrition grinding crosses 200 mesh sieves, obtains shale charcoal sorbing material.
Embodiment 2
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 4% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Grain；
（2）By weight, be 1mol/L zinc chloride by 1 part of mass concentration, 6 parts of Phenoxyethanols, 4 parts of hydroxymethyl celluloses and
2 parts of sodium chloride are added in 20 parts of water, and 1 part of mud granule is added after dissolving, are soaked 1 hour, and soaking temperature is 30 DEG C, is dried；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 800 DEG C, charing heat are warming up to
Solve 15min；
（4）By the hydrochloric acid solution of the concentration 2mol/L containing product in 60 DEG C of water-baths heating response 1min, be washed to neutrality, do
Dry, attrition grinding crosses 200 mesh sieves, obtains shale charcoal sorbing material.
Embodiment 3
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 7% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Grain；
（2）By weight, by zinc chloride, 10 part Phenoxyethanol, 10 part hydroxymethyl celluloses of 2 parts of mass concentrations for 5mol/L
Added with 5 parts of sodium chloride in 30 parts of water, 2 parts of mud granules are added after dissolving, soaked 3 hours, soaking temperature is 50 DEG C, is dried；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 850 DEG C, charing heat are warming up to
Solve 90min；
（4）By the hydrochloric acid solution of the concentration 2mol/L containing product in 80 DEG C of water-baths heating response 3min, be washed to neutrality, do
Dry, attrition grinding crosses 200 mesh sieves, obtains shale charcoal sorbing material.
Embodiment 4
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 5% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Grain；
（2）By weight, be 4mol/L zinc chloride by 1 part of mass concentration, 9 parts of Phenoxyethanols, 8 parts of hydroxymethyl celluloses and
4 parts of sodium chloride are added in 26 parts of water, and 2 parts of mud granules are added after dissolving, are soaked 1.5 hours, and soaking temperature is 38 DEG C, is dried；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 825 DEG C, charing heat are warming up to
Solve 50min；
（4）By the hydrochloric acid solution of the concentration 2mol/L containing product in 74 DEG C of water-baths heating response 1.min, be washed to neutrality,
Grinding is dry, pulverize, 200 mesh sieves is crossed, obtains shale charcoal sorbing material.
Reference examples 1
Difference with embodiment 1 is：Step（2）In be not added with Phenoxyethanol.
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 5% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Grain；
（2）By weight, by zinc chloride, 6 part hydroxymethyl celluloses and 3 part sodium chloride of 1.2 parts of mass concentrations for 3mol/L
Add in 27 parts of water, 1.2 parts of mud granules are added after dissolving, soak 2 hours, soaking temperature is 40 DEG C, is dried；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 830 DEG C, charing heat are warming up to
Solve 50min；
（4）By the hydrochloric acid solution of the concentration 2mol/L containing product in 70 DEG C of water-baths heating response 2min, be washed to neutrality, do
Dry, attrition grinding crosses 200 mesh sieves, obtains shale charcoal sorbing material.
Reference examples 2
Difference with embodiment 2 is：Step（2）In be not added with zinc chloride.
The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, comprises the following steps：
（1）It is 4% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Grain；
（2）By weight, 6 parts of Phenoxyethanols, 4 parts of hydroxymethyl celluloses and 2 parts of sodium chloride are added in 20 parts of water, after dissolving
1 part of mud granule is added, is soaked 1 hour, soaking temperature is 30 DEG C, is dried；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 800 DEG C, charing heat are warming up to
Solve 15min；
（4）By the hydrochloric acid solution of the concentration 2mol/L containing product in 60 DEG C of water-baths heating response 1min, be washed to neutrality, do
Dry, attrition grinding crosses 200 mesh sieves, obtains shale charcoal sorbing material.
Performance test：
| Shale charcoal yield % | Iodine sorption value mg/g | |
| Embodiment 1 | 78 | 640 |
| Embodiment 2 | 77 | 633 |
| Embodiment 3 | 76 | 635 |
| Embodiment 4 | 78 | 638 |
| Reference examples 1 | 57 | 530 |
| Reference examples 2 | 66 | 467 |
As can be seen from the table, shale charcoal yield of the invention is 76~78%, and iodine sorption value is up to 640mg/g, illustrates to utilize this
The method of invention is carried out after immersion treatment to mud granule, can improve the output of final shale charcoal, Phenoxyethanol and oxidation
The adsorption capacity of zinc collaboration enhancing shale charcoal.
It is described above, it is only the present invention preferably specific embodiment, protection scope of the present invention not limited to this is any ripe
Those skilled in the art are known in the technical scope of present disclosure, the letter for the technical scheme that can be become apparent to
Altered or equivalence replacement are each fallen within protection scope of the present invention.
Claims (6)
1. the method that paper-making industrial waste water sludge prepares shale charcoal sorbing material, it is characterised in that comprise the following steps：
（1）It is 4~7% by paper-making industrial waste water sludge condensation, squeezing, drying to moisture content, ground 200 mesh sieve obtains sludge
Particle；
（2）By weight, by 1~2 part of activator, 6~10 parts of Phenoxyethanols, 4~10 parts of hydroxymethyl celluloses and 2~5 parts
Sodium chloride is added in 20~30 parts of water, and 1~2 part of mud granule is added after dissolving, is soaked 1-3 hours, soaking temperature is 30-50
DEG C, dry；
（3）Mud granule after processing is put into pyrolysis oven, nitrogen is passed through as protective gas, 800~850 DEG C are warming up to,
15~90min of charing pyrolysis；
（4）By the hydrochloric acid solution containing product in 60~80 DEG C of water-baths 1~3min of heating response, be washed to neutrality, dry, powder
Breakdown mill, crosses 200 mesh sieves, obtains shale charcoal sorbing material.
2. the method that paper-making industrial waste water sludge according to claim 1 prepares shale charcoal sorbing material, it is characterised in that
Step（1）Moisture content be 5%.
3. the method that paper-making industrial waste water sludge according to claim 1 prepares shale charcoal sorbing material, it is characterised in that
Step（2）In each raw material include：1.2 parts of activators, 8 parts of Phenoxyethanols, 6 parts of hydroxymethyl celluloses, 3 parts of sodium chloride, 27 parts of water
With 1.2 parts of mud granules.
4. the method that paper-making industrial waste water sludge according to claim 1 prepares shale charcoal sorbing material, it is characterised in that
Described activator is the zinc chloride that mass concentration is 1~5mol/L.
5. the method that paper-making industrial waste water sludge according to claim 1 prepares shale charcoal sorbing material, it is characterised in that
Step（3）Reaction temperature be 830 DEG C, the reaction time is 50min.
6. the method that paper-making industrial waste water sludge according to claim 1 prepares shale charcoal sorbing material, it is characterised in that
Step（4）The concentration 2mol/L of middle hydrochloric acid solution.
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| CN201710272297.0A CN106994331A (en) | 2017-04-24 | 2017-04-24 | The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material |
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| CN201710272297.0A CN106994331A (en) | 2017-04-24 | 2017-04-24 | The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111889075A (en) * | 2020-08-05 | 2020-11-06 | 辽宁大学 | Activated carbon adsorbent prepared from papermaking sludge and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844071A (en) * | 2010-05-26 | 2010-09-29 | 高永宏 | Absorption material prepared from paper making mud |
| CN101961644A (en) * | 2010-09-27 | 2011-02-02 | 山东大学 | Chloride-carbonaceous skeleton composite adsorbent and preparation method thereof |
| CN102205964A (en) * | 2011-04-25 | 2011-10-05 | 山东大学 | Granular activated carbon filler for paper mill sludge and preparation method thereof |
| CN104624153A (en) * | 2014-12-09 | 2015-05-20 | 邹仕放 | Method for preparingadsorbing material by utilizing sludge |
| CN105126756A (en) * | 2015-09-09 | 2015-12-09 | 陕西科技大学 | Preparation method for papermaking argillaceous activated carbon adsorption material |
-
2017
- 2017-04-24 CN CN201710272297.0A patent/CN106994331A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844071A (en) * | 2010-05-26 | 2010-09-29 | 高永宏 | Absorption material prepared from paper making mud |
| CN101961644A (en) * | 2010-09-27 | 2011-02-02 | 山东大学 | Chloride-carbonaceous skeleton composite adsorbent and preparation method thereof |
| CN102205964A (en) * | 2011-04-25 | 2011-10-05 | 山东大学 | Granular activated carbon filler for paper mill sludge and preparation method thereof |
| CN104624153A (en) * | 2014-12-09 | 2015-05-20 | 邹仕放 | Method for preparingadsorbing material by utilizing sludge |
| CN105126756A (en) * | 2015-09-09 | 2015-12-09 | 陕西科技大学 | Preparation method for papermaking argillaceous activated carbon adsorption material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111889075A (en) * | 2020-08-05 | 2020-11-06 | 辽宁大学 | Activated carbon adsorbent prepared from papermaking sludge and preparation method and application thereof |
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Application publication date: 20170801 |