CN106512946A - Preparation method of sludge-based charcoal doped with waste PU shoe material - Google Patents

Preparation method of sludge-based charcoal doped with waste PU shoe material Download PDF

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Publication number
CN106512946A
CN106512946A CN201611189582.8A CN201611189582A CN106512946A CN 106512946 A CN106512946 A CN 106512946A CN 201611189582 A CN201611189582 A CN 201611189582A CN 106512946 A CN106512946 A CN 106512946A
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CN
China
Prior art keywords
sludge
footwear
waste
charcoal
waste materials
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611189582.8A
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Chinese (zh)
Inventor
郑育毅
王玉兰
刘常青
刘文伟
吴春山
王菲凤
赵由才
李家兵
孙启元
谢蓉蓉
汪清环
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Fujian Normal University
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Fujian Normal University
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Publication date
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Priority to CN201611189582.8A priority Critical patent/CN106512946A/en
Publication of CN106512946A publication Critical patent/CN106512946A/en
Pending legal-status Critical Current

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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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4893Residues derived from used synthetic products, e.g. rubber from used tyres

Abstract

The invention relates to a preparation method of sludge-based charcoal doped with a waste PU shoe material. The preparation method is characterized by comprising the following steps: 1, drying sludge to the constant weight, grinding the sludge, sieving the sludge through a 200-mesh sieve, grinding the waste PU shoe material and sieving the waste PU shoe material into a 200-mesh particle material; 2, mixing the sludge and the waste PU shoe material according to the proportion of (1 to 3) to 1 in parts by weight, pyrolyzing the sludge and the waste PU shoe material, introducing nitrogen and warming and heating to 400 to 600 DEG C to obtain a pyrolysis product, wherein the flow velocity of the nitrogen is 100 to 200 mL/min; 3, rinsing the pyrolysis product with 1M hydrochloric acid for 5min; 4, filtering hydrochloric acid out, soaking with deionized water, filtering, drying to the constant weight in an oven in 105 DEG C and finally obtaining the sludge-based charcoal doped with waste PU shoe material. According to the preparation method, the preparation cost of the sludge-based charcoal is saved, the limit of preparing the sludge-based charcoal is overcome, the sludge and the waste shoe material are turned into valuable things, and the quality and the sewage treatment performance of the sludge-based charcoal are improved to a great degree.

Description

A kind of preparation method of the sludge base charcoal of doping PU footwear material waste materials
Technical field
The present invention relates to a kind of sludge base charcoal, more particularly to a kind of sludge base charcoal of doping PU footwear material waste materials Preparation method.
Background technology
Charcoal refers to the biomass remaining material Jing after high temperature pyrolysis under anoxic conditions.Charcoal has larger ratio Surface area and loose structure, with good absorption property, heavy metal, ammonia that can be as sewage disposal adsorbent, in absorption water Nitrogen, phosphate etc..
With Development of China's Urbanization, town sewage plant construction is advanced by leaps and bounds, and municipal sludge is total as sewage disposal by-product Amount also drastically rises, if the mishandling secondary pollution that can cause environment.The process of sludge is disposed has become current environment face The Tough questions for facing.
In municipal sludge contain a certain amount of carbon, can as the raw material for preparing charcoal, but its also because contained by sludge into Point complexity, institute's phosphorus content is relatively low, therefore merely with charcoal quality made by which and performance compared with commercial biological charcoal gap very Greatly, its range of application is also limited significantly with value.
PU footwear material waste materials refer to the sole PU of the leftover bits or discarded shoes of polyurethane PU sole course of processing generation Material.PU footwear material waste materials are reprocessed the fine grained or powder to be formed, is incorporated in sludge, the phosphorus content of sludge can be improved, can be made More preferably, absorption property is more preferably for the sludge base charcoal quality of preparation.
The present invention takes the PU footwear material waste materials that adulterate in sludge to prepare charcoal, improves the adsorptivity of sludge base charcoal Can, while realizing the recycling of sludge and PU footwear material waste materials.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the sludge base charcoal of doping PU footwear material waste materials and application, In a kind of simple exercisable mode, improve the performance of sludge base charcoal, lift its absorption in sewage disposal application and go Dirty ability.
The purpose of the present invention is achieved by the following scheme:
1st, sludge is air-dried under field conditions (factors), is then placed in baking oven and is dried to constant weight in 105 DEG C, is crushed to after removing the debris such as stone 4-8mm, then ground, 200 mesh sieves excessively.PU footwear material waste material Jing special equipments crush, grind, sieve, and become the powder of 200 mesh Material.
2nd, by sludge and PU footwear material waste materials, by weight 1~3:1 ratio is sufficiently mixed, and inserts in atmosphere Muffle furnace Pyrolysis, is passed through nitrogen 15min, is heated to 400-600 DEG C with the programming rate of 10-20 DEG C/min afterwards, maintains temperature to stop 2- After 3h, 80 DEG C of dischargings are heated and are cooled in stopping, being placed on cooling in exsiccator, are obtained thermal decomposition product.The through-flow speed of nitrogen is 100-200 mL/min。
3rd, the thermal decomposition product of step (2) is embathed into 5min with the hydrochloric acid of 1M.
4th, filter off step (3) hydrochloric acid, will solid content deionized water soak 20min after filter, deionized water immersion with Filtration step repeats 5 times, then filter upper thing is put into baking oven dries in 105 DEG C to constant weight, the final doping PU footwear material waste materials that obtain Sludge base charcoal.
PU footwear materials waste material of the present invention refers to the footwear of the leftover bits or discarded shoes of polyurethane PU sole course of processing generation Bottom PU expects.
It is an advantage of the current invention that:
The preparation cost of sludge base charcoal has been saved, the limitation of sludge base charcoal preparation has been overcome so that sludge and footwear Material waste material is turned waste into wealth, while largely improving the quality and sewage disposal performance of sludge base charcoal.
Specific embodiment
Embodiment 1
(1) municipal sludge for coming will be fetched(Moisture content 78%)Air-dry under field conditions (factors), then place baking oven and go in 105 DEG C of bakings Moisture, until cooling is taken out after constant weight, removes the debris such as stone cleaning, with crusher in crushing to 4-8mm then ground, 200 mesh excessively Sieve.PU footwear material waste material Jing special equipments crush, grind, sieve, and become the dusty material of 200 mesh.
(2) sludge and each 50g even blend of PU footwear material waste materials of 200 eye mesh screens will be crossed.
(3) material of step (2) even blend is put into into the process of atmosphere Muffle furnace high temperature pyrolysis.It is first fast with 200mL/min Rate is passed through nitrogen 15min, then starts to warm up heating, so that 10 DEG C/min programming rates are to 400 DEG C and keep temperature 3h, closes Heating system is allowed to Temperature fall to 80 DEG C, takes out material and is placed on cooling in exsiccator, obtains thermal decomposition product.
(4) after thermal decomposition product is cooled to room temperature, 5min is embathed with the hydrochloric acid of 1M.
(5) hydrochloric acid is filtered off, filtering residue deionized water is soaked, filtered after stirring and washing 15min, the deionization being repeated 5 times Water logging is washed and filtration step.Filter upper thing is put into baking oven finally to dry in 105 DEG C to constant weight, to be taken out and this is obtained after being dried cooling The sludge base charcoal finished product of doping PU footwear material waste materials prepared by embodiment.
Determination of iodine value:Using the sludge base charcoal prepared by the present embodiment step, its iodine number is with specific surface area by simple 301.1mg/g, the 245.3m for the sludge base charcoal prepared using municipal sludge2/ g brings up to 511.4mg/g, 498.3m2/g。
The application of sewage disposal:Weigh finished product obtained by 2g steps (5), phosphorus-containing wastewater of the input equipped with 1L electromechanics polishing processes In, stirring reaction postprecipitation takes supernatants after precipitation and determines its corresponding water quality index, shows that the doping PU footwear materials of the present embodiment are given up Material COD of the sludge base charcoal to the waste waterCr, TN and TP clearances be respectively 54.5%, 23.0% and 97.4%, it is relatively simple to adopt Made by municipal sludge, sludge base charcoal improves 16.4%, 6.5% and 16.3% respectively.
Municipal sludge described in the present embodiment is taken from:Fuzhou City city sewage treatment plant.
Embodiment 2
(1) municipal sludge for coming will be fetched(Moisture content 72%)Air-dry under field conditions (factors), then place baking oven and go in 105 DEG C of bakings Moisture, until cooling is taken out after constant weight, removes the debris such as stone cleaning, with crusher in crushing to 4-8mm then ground, 200 mesh excessively Sieve.PU footwear material waste material Jing special equipments crush, grind, sieve, and become the dusty material of 200 mesh.
(2) the 100g sludge and 50gPU footwear material waste material even blend of 200 eye mesh screens will be crossed.
(3) step (2) even blend material is put into into the process of atmosphere Muffle furnace high temperature pyrolysis.First with 150mL/min speed Nitrogen 15min is passed through, heating is then started to warm up, so that 15 DEG C/min programming rates are to 500 DEG C and keep temperature 2.5h, is closed Heating system is allowed to Temperature fall to 80 DEG C, takes out material and is placed on cooling in exsiccator, obtains thermal decomposition product.
(4) after thermal decomposition product is cooled to room temperature, 5min is embathed with the hydrochloric acid of 1M.
(5) hydrochloric acid is filtered off, filtering residue deionized water is soaked, filtered after stirring and washing 15min, the deionization being repeated 5 times Water logging is washed and filtration step.Filter upper thing is put into baking oven finally to dry in 105 DEG C to constant weight, to be taken out and this is obtained after being dried cooling The sludge base charcoal finished product of doping PU footwear material waste materials prepared by embodiment.
Determination of iodine value:Using the sludge base charcoal prepared by the present embodiment step, its iodine number is with specific surface area by simple 253.7mg/g, the 205.3m for the sludge base charcoal prepared using municipal sludge2/ g brings up to 453.8mg/g, 419.9m2/g。
The application of sewage disposal:Weigh finished product obtained by 2g steps (5), phosphorus-containing wastewater of the input equipped with 1L electromechanics polishing processes In, stirring reaction postprecipitation takes supernatants after precipitation and determines its corresponding water quality index, shows that the doping PU footwear materials of the present embodiment are given up Material COD of the sludge base charcoal to the waste waterCr, TN and TP clearances be respectively 50.4%, 21.1% and 93.8%, it is relatively simple to adopt Made by municipal sludge, sludge base charcoal improves 13.0%, 4.8% and 13.1% respectively.
Municipal sludge described in the present embodiment is taken from:Fuzhou City city sewage treatment plant.
Embodiment 3
(1) municipal sludge for coming will be fetched(Moisture content 80%)Air-dry under field conditions (factors), then place baking oven and go in 105 DEG C of bakings Moisture, until cooling is taken out after constant weight, removes the debris such as stone cleaning, with crusher in crushing to 4-8mm then ground, 200 mesh excessively Sieve.PU footwear material waste material Jing special equipments crush, grind, sieve, and become the dusty material of 200 mesh.
(2) the 150g sludge and 50gPU footwear material waste material even blend of 200 eye mesh screens will be crossed.
(3) step (2) mixing material is put into into the process of atmosphere Muffle furnace high temperature pyrolysis.First it is passed through with 100mL/min speed Nitrogen 15min, then starts to warm up heating, so that 20 DEG C/min programming rates are to 600 DEG C and keep temperature 2h, closes heating system System is allowed to Temperature fall to 80 DEG C, takes out material and is placed on cooling in exsiccator, obtains thermal decomposition product.
(4) after thermal decomposition product is cooled to room temperature, 5min is embathed with the hydrochloric acid of 1M.
(5) hydrochloric acid is filtered off, filtering residue deionized water is soaked, filtered after stirring and washing 15min, the deionization being repeated 5 times Water logging is washed and filtration step.Filter upper thing is put into baking oven finally to dry in 105 DEG C to constant weight, to be taken out and this is obtained after being dried cooling The sludge base charcoal finished product of doping PU footwear material waste materials prepared by embodiment.
Determination of iodine value:Using the sludge base charcoal prepared by the present embodiment step, its iodine number is with specific surface area by simple 215.2mg/g, the 163.3m for the sludge base charcoal prepared using municipal sludge2/ g, brings up to 401.6mg/g, 342.7m2/g。
The application of sewage disposal:Weigh finished product obtained by 2g steps (5), phosphorus-containing wastewater of the input equipped with 1L electromechanics polishing processes In, stirring reaction postprecipitation takes supernatants after precipitation and determines its corresponding water quality index, shows that the doping PU footwear materials of the present embodiment are given up Material COD of the sludge base charcoal to the waste waterCr, TN and TP clearances be respectively 44.2%, 18.5% and 86.2%, it is relatively simple to adopt Made by municipal sludge, sludge base charcoal improves 10.2%, 4.4% and 11.0% respectively.
Municipal sludge described in the present embodiment is taken from:Fuzhou City city sewage treatment plant.

Claims (4)

1. a kind of sludge base charcoal preparation method of doping PU footwear material waste materials, is characterized in that:
1) sludge is air-dried under field conditions (factors), is then placed in baking oven and is dried to constant weight in 105 DEG C, is crushed to after removing the debris such as stone 4-8mm, then ground, 200 mesh sieves excessively;PU footwear material waste material Jing special equipments crush, grind, sieve, and become the powder of 200 mesh Material;
2)By step 1)Described sludge and PU footwear material waste materials, by weight 1~3:1 ratio is sufficiently mixed, and inserts atmosphere It is pyrolyzed in Muffle furnace, is passed through nitrogen 15min, is heated to 400-600 DEG C and obtains thermal decomposition product;
3)By stepThermal decomposition product embathe 5min with the hydrochloric acid of 1M, filter off hydrochloric acid, solid content deionized water soaked Filter after 20min, deionized water immersion is repeated 5 times with filtration step, then filter upper thing is put into baking oven and dry to perseverance in 105 DEG C Weight, the final sludge base charcoal for obtaining doping PU footwear material waste materials.
2. a kind of sludge base charcoal preparation method of doping PU footwear material waste materials according to claim 1, is characterized in that institute The leaching pyrolysis stated, is passed through the nitrogen time for 15min, and the through-flow speed of nitrogen is 100-200 mL/min.
3. a kind of sludge base charcoal preparation method of doping PU footwear material waste materials according to claim 1, is characterized in that institute The pyrolysis stated, programming rate are 10-20 DEG C/min, and after maintaining temperature to stop 2-3h after intensification, stopping is heated and is cooled to 80 DEG C discharging, is placed on cooling in exsiccator.
4. a kind of sludge base charcoal preparation method of doping PU footwear material waste materials according to claim 1, is characterized in that institute The PU footwear material waste materials stated refer to the sole PU material of the leftover bits or discarded shoes of polyurethane PU sole course of processing generation.
CN201611189582.8A 2016-12-21 2016-12-21 Preparation method of sludge-based charcoal doped with waste PU shoe material Pending CN106512946A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107297112A (en) * 2017-07-04 2017-10-27 浙江工业大学 The deodorization of biological sludge pyrolysis synthesis gas and purification processes system
CN109851026A (en) * 2019-01-08 2019-06-07 同济大学 A kind of dye waste water treatment method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103754869A (en) * 2014-01-02 2014-04-30 上海大学 Method for preparing high-quality active carbon by adopting waste polyurethane foamed plastic
CN104258808A (en) * 2014-09-02 2015-01-07 中国科学院城市环境研究所 Method and system for increasing specific surface area of sludge biochar

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN103754869A (en) * 2014-01-02 2014-04-30 上海大学 Method for preparing high-quality active carbon by adopting waste polyurethane foamed plastic
CN104258808A (en) * 2014-09-02 2015-01-07 中国科学院城市环境研究所 Method and system for increasing specific surface area of sludge biochar

Non-Patent Citations (2)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107297112A (en) * 2017-07-04 2017-10-27 浙江工业大学 The deodorization of biological sludge pyrolysis synthesis gas and purification processes system
CN109851026A (en) * 2019-01-08 2019-06-07 同济大学 A kind of dye waste water treatment method

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Application publication date: 20170322