CN109967030A - A kind of ammonia nitrogen absorption material and preparation method thereof - Google Patents

A kind of ammonia nitrogen absorption material and preparation method thereof Download PDF

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Publication number
CN109967030A
CN109967030A CN201711447784.2A CN201711447784A CN109967030A CN 109967030 A CN109967030 A CN 109967030A CN 201711447784 A CN201711447784 A CN 201711447784A CN 109967030 A CN109967030 A CN 109967030A
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Prior art keywords
ammonia nitrogen
absorption
parts
weight
raw
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CN201711447784.2A
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Inventor
狄巧玲
宋艳丽
曹硕文
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Shanghai Shen Fu Biological Technology Co Ltd
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Shanghai Shen Fu Biological Technology Co Ltd
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Priority to CN201711447784.2A priority Critical patent/CN109967030A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • 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
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • 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
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016Particle form
    • B01J20/28019Spherical, ellipsoidal or cylindrical
    • 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
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia

Abstract

The invention discloses a kind of ammonia nitrogen absorption materials, belong to field of waste water treatment.Key step of the invention includes: that 50-60 parts by weight are discarded soil, raw material ball is made after being mixed in 30-40 parts by weight vermiculite, 5-10 parts by weight waterglass, 1-5 parts by weight technical grade NaOH, and is calcined to obtain absorption protocorm at 600-700 DEG C under ventilation state;After absorption protocorm is impregnated in hydrochloric acid solution, ammonia nitrogen absorption material is obtained.The preparation method is creatively raw material using discarded soil, is modified using the NaOH under molten condition to soil;Swelling occurs for the layer structure of vermiculite simultaneously, increases adsorption specific surface area.Preparation method is easy to operate, and resulting materials stability is high, can be applied to the ammonia nitrogen absorption removal in all kinds of waste water.

Description

A kind of ammonia nitrogen absorption material and preparation method thereof
Technical field
The invention belongs to field of waste water treatment, are related to a kind of recycling and reusing of discarded soil in wastewater processing technology Using specially a kind of ammonia nitrogen absorption material and preparation method thereof.
Background technique
With the rapid development of industry, ammonia nitrogen waste water discharge amount is increasingly sharpened.Water eutrophication caused by nitrogen and phosphorus element Problem comes one after another, and the lake blue algaes Breakout events such as Taihu Lake are commonplace.Meanwhile in ammonia nitrogen in high density water body, ammonia nitrogen again may be used It is toxic nitrate nitrogen, nitrite nitrogen etc. by microorganism conversion, has biggish toxic action to human body and organism in water, then Influence aquatic organism breeding and existence.A few days ago, it is increasingly taken seriously to the processing of high-concentration ammonia nitrogenous wastewater.The minimizing technology of ammonia nitrogen is very It is more, mainly there are bioanalysis, chemical method, absorption and ion-exchange etc. at present.Absorption and ion-exchange due to occupied area is small, Simple process and it is easy to operate the advantages that, be commonly used for the processing of ammonia nitrogen waste water.Zeolite molecular sieve relies on its adsorptivity outstanding Energy (adsorption and ion-exchange selectivity), makes it be widely used in adsorbing separation.At present to natural zeolite and modification Natural zeolite goes ammonia nitrogen studies in water removal a lot of.For using the research that discarded soil is raw material preparation ammonia nitrogen absorption material fresh It has been reported that.
Summary of the invention
It is of the invention innovative creatively using soil is discarded as raw material, soil is carried out using the NaOH under molten condition It is modified;Swelling occurs for the layer structure of vermiculite simultaneously, and interlamellar spacing becomes larger.This preparation method is easy to operate, and resulting materials combine The swelling structure of the biggish porosity of soil and vermiculite increases adsorption specific surface area, improves ammonia nitrogen absorption performance.It can be applied to each Ammonia nitrogen absorption removal in class waste water.
A kind of preparation method of ammonia nitrogen absorption material comprising following steps:
(a) 50-60 parts by weight are weighed and discard soil, 30-40 parts by weight vermiculite, 5-10 parts by weight waterglass, 1-5 parts by weight Part technical grade NaOH, mixing;
(b) it is crushed in pulverizer, is sieved, obtains mixture uniformly mixed, that granularity is small;
(c) raw material ball is made in the mixture for obtaining step (b) on facility for granulating;
(d) raw material ball obtained by step (c) is put into electric furnace, under ventilation condition, is warming up to 600-700 DEG C, keeps After 1.5h-3h, stop heating, continue to keep ventilation, be down to room temperature with furnace, obtains absorption protocorm;
(e) the absorption protocorm that step (d) obtains is put into hydrochloric acid and impregnates the 1h acquisition ammonia nitrogen absorption material.
Preferably,
Sieving was 80 meshes described in step (b);
The diameter of step (c) raw material ball is 1~3mm of diameter;
Step (d) the ventilation wind speed is 7-10m3/h;Heating rate is 3~10 DEG C/min, preferably 5 DEG C/min;
The molar concentration of step (e) hydrochloric acid is 0.5-2mol/L.
The discarded soil is crops excess contamination soil, the discarded soil of factory.
The invention also discloses ammonia nitrogen absorption materials prepared by the above method.
The invention also discloses the application of the ammonia nitrogen absorption material in the treatment of waste water, specially inhale in the treatment of waste water The application of attached ammonia nitrogen.
Beneficial effect
Compared to more traditional zeolitic material as ammonia nitrogen adsorbent, using discarded soil as raw material, raw material is cheap and easy to get, benefit In reducing cost.In addition, natural zeolite adsorption efficiency is low, can generally chemical modification be carried out to zeolite, be then sintered Ball processed can be just able to using further improving its application cost.Tool is directly prepared by a step sintering process in this patent There is the soil ball of some strength, it is easy to operate, it is conducive to industrialized production.And have certain recycling to waste, be conducive to ring The sustainable development of border safeguard industries and agricultural.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but the present invention is special The content of benefit is not limited solely to the following examples.
Embodiment 1
(a) 60 parts by weight are weighed and discard soil, 30 parts by weight vermiculites, 5 parts by weight waterglass, 5 parts by weight technical grade NaOH Ratio, mixing;
(b) it is crushed in pulverizer, and crosses 80 meshes, obtain mixture uniformly mixed, that granularity is small;
(c) raw material ball that diameter is 2mm or so is made in the mixture that step (b) obtains on granulator;
(d) raw material ball obtained by step (c) is put into electric furnace, is 10m in ventilation wind speed3Under/h condition, with 5 DEG C/min liter Temperature is to 650 DEG C, after keeping 2h, stops heating, continues to keep ventilation, is down to room temperature with furnace, obtains absorption protocorm;
(e) the absorption protocorm that step (d) obtains is impregnated into the hydrochloric acid of 1.5mol/L 1h and obtains ammonia nitrogen absorption material.
Embodiment 2
(a) 50 parts by weight are weighed and discard soil, 35 parts by weight vermiculites, 10 parts by weight waterglass, 5 parts by weight technical grades NaOH, mixing;
(b) it is crushed in pulverizer, and crosses 80 meshes, obtain mixture uniformly mixed, that granularity is small;
(c) mixture that step (b) obtains is made to the raw material ball of diameter 2mm or so on granulator;
(d) raw material ball obtained by step (c) is put into electric furnace, is 7m in ventilation wind speed3Under/h condition, with 5 DEG C/min liter Temperature is to 700 DEG C, after keeping 1.5h, stops heating, continues to keep ventilation, is down to room temperature with furnace, obtains absorption protocorm;
(e) the absorption protocorm that step (d) obtains is impregnated into the hydrochloric acid of 2mol/L 1h and obtains ammonia nitrogen absorption material.
Embodiment 3
(a) 55 parts by weight are weighed and discard soil, 30 parts by weight vermiculites, 10 parts by weight waterglass, 5 parts by weight technical grades NaOH, mixing;
(b) it is crushed in pulverizer, and crosses 80 meshes, obtain mixture uniformly mixed, that granularity is small;
(c) step (b) is obtained into the raw material ball that diameter 2mm or so is made in mixture on granulator;
(d) raw material ball obtained by step (c) is put into electric furnace, is 10m in ventilation wind speed3Under/h condition, with 5 DEG C/min liter Temperature is to 600 DEG C, after keeping 3h, stops heating, continues to keep ventilation, is down to room temperature with furnace, obtains absorption protocorm;
(e) the absorption protocorm that step (d) obtains is impregnated into the hydrochloric acid of 2mol/L 1h and obtains ammonia nitrogen absorption material.
Embodiment 4
(a) weigh 60 parts by weight discard soil, 30 parts by weight vermiculites, 7 parts by weight waterglass, 3 parts by weight technical grade NaOH, Mixing;
(b) it is crushed in pulverizer, and crosses 80 meshes, obtain mixture uniformly mixed, that granularity is small;
(c) step (b) is obtained into the raw material ball that diameter 2mm or so is made in mixture on granulator;
(d) raw material ball obtained by step (c) is put into electric furnace, is 10m in ventilation wind speed3Under/h condition, with 5 DEG C/min liter Temperature is to 650 DEG C, after keeping 2.5h, stops heating, continues to keep ventilation, is down to room temperature with furnace, obtains absorption protocorm;
(e) the absorption protocorm that step (d) obtains is impregnated into the hydrochloric acid of 1.5mol/L 1h and obtains ammonia nitrogen absorption material.
Test case 1
The ammonia nitrogen absorption material that embodiment 1-4 is obtained is tested for the property.
The adsorbent material for taking the embodiment 1-4 of 0.4g respectively, being respectively implanted 200mL concentration is 6.0mol/L ammonia nitrogen solution In, adsorption experiment is carried out in shaken cultivation case.After adsorbing 2h, with 0.45 μm of membrane filtration, it is dense to measure remaining ammonia nitrogen in filtrate Degree.
The measurement of ammonia-nitrogen content uses national standard " water quality/ammonia nitrogen measurement/Berthelot spectrophotometry " (HJ535-2009), and ammonia nitrogen absorption removal rate is calculated as follows:
R=(c0–c1)/c0× 100%
In formula: r is ammonia nitrogen absorption removal rate, %;c0For initial ammonia nitrogen concentration, mol/L;
c1For remaining ammonia nitrogen concentration, mol/L
Each embodiment is all provided with parallel test three times, is averaged.

Claims (8)

1. a kind of preparation method of ammonia nitrogen absorption material, which comprises the steps of:
(a) 50-60 parts by weight are weighed and discard soil, 30-40 parts by weight vermiculite, 5-10 parts by weight waterglass, 1-5 parts by weight work Industry grade NaOH, mixing;
(b) it is crushed in pulverizer, is sieved, obtains mixture uniformly mixed, that granularity is small;
(c) raw material ball is made in the mixture for obtaining step (b) on facility for granulating;
(d) raw material ball obtained by step (c) is put into electric furnace, under ventilation condition, is warming up to 600-700 DEG C, keeps 1.5h-3h Afterwards, stop heating, continue to keep ventilation, be down to room temperature with furnace, obtain absorption protocorm;
(e) the absorption protocorm that step (d) obtains is put into hydrochloric acid and impregnates the 1h acquisition ammonia nitrogen absorption material.
2. preparation method as described in claim 1, it is characterised in that: sieving was 80 meshes described in step (b).
3. preparation method as described in claim 1, it is characterised in that: the diameter of step (c) raw material ball be diameter 1~ 3mm。
4. preparation method as described in claim 1, it is characterised in that: step (d) the ventilation wind speed is 7-10m3/h;Heating Speed is 3~10 DEG C/min.
5. preparation method as described in claim 1, it is characterised in that: the molar concentration of step (e) hydrochloric acid is 0.5- 2mol/L。
6. the ammonia nitrogen absorption material that preparation method described in any one of -5 obtains according to claim 1.
7. the application of ammonia nitrogen absorption material as claimed in claim 6 in the treatment of waste water.
8. the application that ammonia nitrogen absorption material as claimed in claim 6 adsorbs ammonia nitrogen in the treatment of waste water.
CN201711447784.2A 2017-12-27 2017-12-27 A kind of ammonia nitrogen absorption material and preparation method thereof Pending CN109967030A (en)

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