CN109499553A - A kind of dyeing and printing sewage processing porous spheroidal adsorbent and preparation method thereof - Google Patents
A kind of dyeing and printing sewage processing porous spheroidal adsorbent and preparation method thereof Download PDFInfo
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- CN109499553A CN109499553A CN201811572703.6A CN201811572703A CN109499553A CN 109499553 A CN109499553 A CN 109499553A CN 201811572703 A CN201811572703 A CN 201811572703A CN 109499553 A CN109499553 A CN 109499553A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid 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
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid 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 surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The present invention provides a kind of dyeing and printing sewage processing porous spheroidal adsorbent and preparation method thereof, it is related to technology of waste water control field, the adsorbent is as made by the compound rear cyanurotriamide modified almandine of incorporation of sodium alginate and oxidized porous starch, the present invention combines organic adsorption material and inorganic adsorbing material, also there is very high adsorption activity at low temperature, energy consumption can be reduced, process performance is improved, there is good adsorption effect to contents of many kinds of heavy metal ion and organic matter.
Description
Technical field
The present invention relates to technology of waste water control fields, and in particular to a kind of dyeing and printing sewage handle porous spheroidal adsorbent and
Preparation method.
Background technique
Dyeing and printing sewage be to process cotton, fiber crops, chemical fibre and its blending product, the printing and dyeing based on silk, woolens dyeing and finishing and
The waste water of the discharges such as silk mill.Kinds of fibers and processing technology difference, the water and water quality of dyeing and printing sewage are also different.Wherein, it prints
Dyeing mill wastewater water is larger, every dyeing and printing process 1t textile water consumption 100-200t, and wherein 80-90% is discharged as waste water.Printing and dyeing
Sewage has the characteristics that water is big, organic pollutant content is high, alkalinity is big, change of water quality is big, belong to intractable industrial wastewater it
One, containing pollutants such as dyestuff, slurry, auxiliary agent, finish, soda acid, fiber impurity, sand substance, inorganic salts in dyeing and printing sewage, more
Serious also carcinogenic and teratogenesis organic compound, has virose heavy metal etc., direct emission environmental pollution is serious.Print
Contaminate one kind of more refractory reason in waste water category industrial wastewater.Due to technology, economy etc., the life object-object of current most of uses
Reason administering method can only achieve basic emission request.Although being declined slightly in coloration, to organic substance only resolve into compared with
Small substance is difficult control to these decomposition product properties and is also difficult to grasp, not can guarantee and do not generate harm to environment.Dyeing and printing sewage
Processing method mainly has physical method, chemical method and electrolysis method.Wherein chemical method and physical method, which are often used in mixed way, can reach more preferable
Effect.Applying in physical method at most is absorption, is mainly adsorbed using adsorbent to harmful substance, reaches purification
The purpose of water quality.
107758789 A of Chinese patent CN discloses the preparation and its application of a kind of printing and dyeing wastewater treatment agent, preparation step
Suddenly are as follows: coconut shell flour is added in phosphoric acid solution and is impregnated, calcining and activating, is then added copper nitrate solution and cerous nitrate solution is modified,
Calcine to obtain modified cocoanut active charcoal；Deionized water is added in organic modifiers and aluminium chloride, bentonite is added, is ground after reaction
Obtain modified alta-mud；Take modified coconut activated powdered carbon, polyferric chloride, aluminium polychloride, modified alta-mud, cornstarch,
Sodium acetate, polyacrylamide, polysorbate, plant fiber, ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are uniformly mixed, are granulated dirty
Water treatment agent.Have the beneficial effect that and compound each raw material, play coordinative role, can sustainable processing coloration, concentration it is higher
Dyeing and printing sewage, water quality that treated can iterative cycles utilizations；Water treatment agent handles the simple process of dyeing and printing sewage, efficiently, processing
It is at low cost, it is without side-effects to operator.
105582880 A of Chinese patent CN discloses a kind of sewage treatment high-performance bio adsorbent, and the adsorbent is by aoxidizing
Calcium, silica, aluminium oxide, sulfur trioxide, iron oxide, magnesia, titanium dioxide, potassium oxide, manganese oxide, sodium oxide molybdena, water group
At sphere of action extensively using equipment is simplified later, reduces cost of investment, and then improve Business Economic Benefit.The scope of application
It extensively can be used for handling the various sewage from sanitary wastewater to industrial wastewater.The flocculate formed after processing is non-friable, and dehydration property is good,
It being easily handled, the water clarity after effect is high, and water turbidity is almost 0, and precipitable water is recycled, and it is formed and is recycled, section
About water resource.Shut off in the source of sewage of small device and a large amount of processing is concentrated to be used in combination, can thoroughly solve effluent problem, and handle
Self detergent power of water is strong, can reasonable time interior holding detergent power.
Above-mentioned sewage adsorption treatment agent is bad to dyeing and printing sewage treatment effect, is unable to satisfy actual use.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of dyeing and printing sewage processing porous spheroidal adsorbent and its systems
Preparation Method.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of porous spheroidal adsorbent of dyeing and printing sewage processing, the adsorbent is by sodium alginate and oxidized porous starch
After compound made by the cyanurotriamide modified almandine of incorporation.
Above-mentioned dyeing and printing sewage handles the preparation method of porous spheroidal adsorbent, comprising the following steps:
(1) tapioca is add to deionized water, sodium hydroxide solution is added and adjusts pH to 8-10, is heated to 90-
It after 95 DEG C of stirring 50-80min, is cooled to 40-50 DEG C and adds oxidant and ferric sulfate, continue to stir 1-3h, by three metaphosphoric acids
After stirring 10-20min is added in sodium and Macrogol 6000, sodium alginate and Span80 are added, continued after stirring 10-20min
5-10h is stood, is slowly dumped into calcium chloride solution, 5-8h, the solid collected are reacted, washing, ethyl alcohol wash rear 50-60
DEG C drying, obtain A material；
(2) 400 meshes are crossed after almandine being pulverized, and are added in the ethanol solution of melamine, 50-60 DEG C is stirred
It after mixing 1-6h, filters, under 130-150 DEG C of nitrogen protection of solid material after dry 5-10h, is warming up to 800-1050 DEG C of calcining 1-2h,
Obtain B material；
(3) it is added in ethanol solution after mixing A material, B mechanical mass, at room temperature drips the acetic acid solution of chitosan
After adding, it being warming up to 35-40 DEG C of stirring 1-5h, mixture is placed in flask, Rotary Evaporators vacuum distillation removes solvent,
120-150 DEG C of drying after neutrality is washed to after solid material is poured out.
Preferably, the mass concentration of sodium hydroxide solution is 5-20% in step (1).
Preferably, oxidant is hydrogen peroxide or sodium hypochlorite in step (1).
Preferably, the mass ratio of the quality of ferric sulfate and tapioca is 1:15-40 in step (1).
Preferably, the mass ratio of Macrogol 6000 and tapioca is 1:20-25 in step (1).
Preferably, the mass concentration of calcium chloride solution is 0.5-2.5% in step (1).
Preferably, the mass concentration of the ethanol solution of melamine is 20-30% in step (2).
Preferably, A material in step (3), B material mass ratio be 4-8:1.
Preferably, the mass concentration of the acetic acid solution of chitosan is 10-15% in step (3).
(3) beneficial effect
The present invention provides a kind of dyeing and printing sewages to handle porous spheroidal adsorbent and preparation method thereof, has beneficial below
Effect:
Starch is needed in molecule containing active base and sugared former times key by the limitation of ative starch property as macromolecule polymer
It just can be used as adsorbent through processing to use, the complexity and particularity of starch structure, such as the diversity of dentate, surface area is small,
Porosity is weak etc., causes it poor to the adsorptivity of metal ion in dyeing and printing sewage and organic matter, it is difficult to meet dyeing and printing sewage and control
The practical application of reason will make adsorbent and seldom be seen in report (Mianyang Teachers College's chemistry and chemical engineering science after starch oxidation
Huanghai Sea rosy clouds, Zhang Ying, Zhang Xueqin of institute have studied oxidized starch to Cd2+Absorption property), the present invention in oxidized porous starch work
It is adsorbent main body by the way that sodium alginate is added, the compactness of oxidized porous starch can be improved, promoted to metal ion and had
The absorption property of machine object, and cyanurotriamide modified almandine is mixed, almandine itself is nesosilicate mineral,
Itself is to heavy metal ion Cu2+And Pb2+There is a very strong adsorptivity, with after melamine-impregnated under high temperature, surface nitrogen content and contains
Nitrogen functional group increases, the adsorbing and removing performance boost to organic matter, and melamine penetrates into almandine powder, with forging
Burn gradually to decompose in release, can promote the internal gutter structure of almandine powder, promote surface area, and the present invention is by organic suction
Enclosure material and inorganic adsorbing material combine, and also have very high adsorption activity at low temperature, it is possible to reduce energy consumption, raising processing
Performance has good adsorption effect to contents of many kinds of heavy metal ion and organic matter.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 15% is added and adjusts pH to 8-
10, after being heated to 92 DEG C of stirring 70min, it is cooled to 48 DEG C and adds hydrogen peroxide and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:30), continue to stir 2.5h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and wood
The mass ratio of sweet potato starch is 1:20) stirring 18min is added after, sodium alginate and Span80 are added, continue to stir quiet after 10min
6h is set, is slowly dumped into the calcium chloride solution that mass concentration is 2.5%, 6h, the solid collected, washing, second are reacted
55 DEG C of drying after alcohol is washed, obtain A material；400 meshes are crossed after almandine is pulverized, being added to mass concentration is 20%
It in the ethanol solution of melamine, after 55 DEG C of stirring 2h, filters, under 130 DEG C of nitrogen protections of solid material after dry 10h, is warming up to
950 DEG C of calcining 1h, obtain B material；It will be added in ethanol solution after A material, B material 6:1 mechanical mixture in mass ratio, room temperature
After entrance is added dropwise in the acetic acid solution of the lower chitosan for being 10% by mass concentration, 35 DEG C of stirring 4h are warming up to, mixture is placed in
In flask, Rotary Evaporators vacuum distillation removes solvent, and 140 DEG C of drying after neutrality are washed to after solid material is poured out.
Embodiment 2:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 20% is added and adjusts pH to 8-
10, after being heated to 90 DEG C of stirring 60min, it is cooled to 40 DEG C and adds hydrogen peroxide and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:30), continue to stir 3h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 15min is added for 1:20) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 10min
7h is slowly dumped into the calcium chloride solution that mass concentration is 1.5%, reacts 6h, the solid collected, washing, ethyl alcohol
50 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 25%
It in the ethanol solution of poly cyanamid, after 50 DEG C of stirring 1h, filters, under 130 DEG C of nitrogen protections of solid material after dry 6h, is warming up to 800
DEG C calcining 1h, obtain B material；It will be added in ethanol solution after A material, B material 4:1 mechanical mixture in mass ratio, at room temperature
After entrance is added dropwise for the acetic acid solution of 12% chitosan in mass concentration, 35 DEG C of stirring 1h are warming up to, mixture is placed in burning
In bottle, Rotary Evaporators vacuum distillation removes solvent, and 120 DEG C of drying after neutrality are washed to after solid material is poured out.
Embodiment 3:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 5% is added and adjusts pH to 8-
10, after being heated to 95 DEG C of stirring 80min, it is cooled to 50 DEG C and adds hydrogen peroxide and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:20), continue to stir 1h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 18min is added for 1:20) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 15min
10h is slowly dumped into the calcium chloride solution that mass concentration is 0.5%, reacts 8h, the solid collected, washing, ethyl alcohol
50 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 20%
It in the ethanol solution of poly cyanamid, after 50 DEG C of stirring 2h, filters, under 145 DEG C of nitrogen protections of solid material after dry 5h, is warming up to 800
DEG C calcining 2h, obtain B material；It will be added in ethanol solution after A material, B material 8:1 mechanical mixture in mass ratio, at room temperature
After entrance is added dropwise for the acetic acid solution of 15% chitosan in mass concentration, 38 DEG C of stirring 5h are warming up to, mixture is placed in burning
In bottle, Rotary Evaporators vacuum distillation removes solvent, and 135 DEG C of drying after neutrality are washed to after solid material is poured out.
Embodiment 4:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 5% is added and adjusts pH to 8-
10, after being heated to 90 DEG C of stirring 50min, it is cooled to 40 DEG C and adds hydrogen peroxide and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:15), continue to stir 1h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 10min is added for 1:20) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 10min
5h is slowly dumped into the calcium chloride solution that mass concentration is 0.5%, reacts 5h, the solid collected, washing, ethyl alcohol
50 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 20%
It in the ethanol solution of poly cyanamid, after 50 DEG C of stirring 1h, filters, under 130 DEG C of nitrogen protections of solid material after dry 5h, is warming up to 800
DEG C calcining 1h, obtain B material；It will be added in ethanol solution after A material, B material 4:1 mechanical mixture in mass ratio, at room temperature
After entrance is added dropwise for the acetic acid solution of 10% chitosan in mass concentration, 35 DEG C of stirring 1h are warming up to, mixture is placed in burning
In bottle, Rotary Evaporators vacuum distillation removes solvent, and 120 DEG C of drying after neutrality are washed to after solid material is poured out.
Embodiment 5:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 20% is added and adjusts pH to 8-
10, after being heated to 95 DEG C of stirring 80min, it is cooled to 50 DEG C and adds sodium hypochlorite and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:40), continue to stir 3h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 20min is added for 1:25) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 20min
10h is slowly dumped into the calcium chloride solution that mass concentration is 2.5%, reacts 8h, the solid collected, washing, ethyl alcohol
60 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 30%
It in the ethanol solution of poly cyanamid, after 60 DEG C of stirring 6h, filters, under 150 DEG C of nitrogen protections of solid material after dry 10h, is warming up to
1050 DEG C of calcining 2h, obtain B material；It will be added in ethanol solution after A material, B material 8:1 mechanical mixture in mass ratio, room
After entrance is added dropwise in the acetic acid solution for the chitosan for being 15% by mass concentration under temperature, 40 DEG C of stirring 5h are warming up to, mixture is set
In in flask, Rotary Evaporators vacuum distillation removes solvent, and 150 DEG C of drying are i.e. after neutrality is washed to after solid material is poured out
It can.
Embodiment 6:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 18% is added and adjusts pH to 8-
10, after being heated to 92 DEG C of stirring 55min, it is cooled to 50 DEG C and adds hydrogen peroxide and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:35), continue to stir 1h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 20min is added for 1:20) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 10min
10h is slowly dumped into the calcium chloride solution that mass concentration is 0.5%, reacts 8h, the solid collected, washing, ethyl alcohol
55 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 30%
It in the ethanol solution of poly cyanamid, after 50 DEG C of stirring 5h, filters, under 135 DEG C of nitrogen protections of solid material after dry 5h, is warming up to 850
DEG C calcining 2h, obtain B material；It will be added in ethanol solution after A material, B material 4:1 mechanical mixture in mass ratio, at room temperature
After entrance is added dropwise for the acetic acid solution of 10% chitosan in mass concentration, 40 DEG C of stirring 2h are warming up to, mixture is placed in burning
In bottle, Rotary Evaporators vacuum distillation removes solvent, and 120 DEG C of drying after neutrality are washed to after solid material is poured out.
Embodiment 7:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 5% is added and adjusts pH to 8-
10, after being heated to 95 DEG C of stirring 50min, it is cooled to 50 DEG C and adds hydrogen peroxide and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:40), continue to stir 1h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 10min is added for 1:25) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 20min
5h is slowly dumped into the calcium chloride solution that mass concentration is 2.5%, reacts 5h, the solid collected, washing, ethyl alcohol
60 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 20%
It in the ethanol solution of poly cyanamid, after 60 DEG C of stirring 1h, filters, under 150 DEG C of nitrogen protections of solid material after dry 5h, is warming up to 1050
DEG C calcining 1h, obtain B material；It will be added in ethanol solution after A material, B material 8:1 mechanical mixture in mass ratio, at room temperature
After entrance is added dropwise for the acetic acid solution of 10% chitosan in mass concentration, 40 DEG C of stirring 1h are warming up to, mixture is placed in burning
In bottle, Rotary Evaporators vacuum distillation removes solvent, and 150 DEG C of drying after neutrality are washed to after solid material is poured out.
Embodiment 8:
A kind of dyeing and printing sewage handle porous spheroidal adsorbent the preparation method is as follows:
Tapioca is add to deionized water, the sodium hydroxide solution that mass concentration is 20% is added and adjusts pH to 8-
10, after being heated to 90 DEG C of stirring 80min, it is cooled to 40 DEG C and adds sodium hypochlorite and ferric sulfate (quality of ferric sulfate and cassava
The mass ratio of starch is 1:15), continue to stir 3h, by sodium trimetaphosphate and Macrogol 6000 (Macrogol 6000 and cassava
After stirring 20min is added for 1:20) in the mass ratio of starch, sodium alginate and Span80 are added, continue to stand after stirring 10min
10h is slowly dumped into the calcium chloride solution that mass concentration is 0.5%, reacts 8h, the solid collected, washing, ethyl alcohol
50 DEG C of drying, obtain A material after washing；400 meshes are crossed after almandine is pulverized, and are added to three that mass concentration is 30%
It in the ethanol solution of poly cyanamid, after 50 DEG C of stirring 6h, filters, under 130 DEG C of nitrogen protections of solid material after dry 10h, is warming up to 800
DEG C calcining 2h, obtain B material；It will be added in ethanol solution after A material, B material 4:1 mechanical mixture in mass ratio, at room temperature
After entrance is added dropwise for the acetic acid solution of 15% chitosan in mass concentration, 35 DEG C of stirring 5h are warming up to, mixture is placed in burning
In bottle, Rotary Evaporators vacuum distillation removes solvent, and 120 DEG C of drying after neutrality are washed to after solid material is poured out.
The following table 1 is 1-3 of embodiment of the present invention adsorbent to the absorption property of methyl blue dye and the result of temperature:
It is respectively configured 6 parts of methyl blue dyes when test, concentration is 10mg/L, after 2h, the concentration of methyl blue dye is measured,
Calculate adsorption rate.
Table 1:
By upper table 1 it is found that adsorbent of the present invention also has very high adsorption activity to methyl blue dye at low temperature, due to print
The processing for staining water can reduce energy consumption, improve process performance.
The following table 2 is absorption property result of 1-3 of the embodiment of the present invention adsorbent to heavy metal ion and organic matter:
Table 2:
By upper table 2 it is found that adsorbent of the present invention has good adsorption effect to contents of many kinds of heavy metal ion and organic matter.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of dyeing and printing sewage handles porous spheroidal adsorbent, which is characterized in that the adsorbent is by sodium alginate and oxygen
Change made by the compound rear cyanurotriamide modified almandine of incorporation of porous-starch.
2. the preparation method that dyeing and printing sewage as described in claim 1 handles porous spheroidal adsorbent, which is characterized in that including
Following steps:
(1) tapioca is add to deionized water, sodium hydroxide solution is added and adjusts pH to 8-10, is heated to 90-95 DEG C
After stirring 50-80min, be cooled to 40-50 DEG C and add oxidant and ferric sulfate, continue to stir 1-3h, by sodium trimetaphosphate and
After stirring 10-20min is added in Macrogol 6000, sodium alginate and Span80 are added, continue to stand after stirring 10-20min
5-10h is slowly dumped into calcium chloride solution, reacts 5-8h, the solid collected, and rear 50-60 DEG C of baking is washed in washing, ethyl alcohol
It is dry, obtain A material；
(2) 400 meshes are crossed after almandine being pulverized, and are added in the ethanol solution of melamine, 50-60 DEG C of stirring 1-
It after 6h, filters, under 130-150 DEG C of nitrogen protection of solid material after dry 5-10h, is warming up to 800-1050 DEG C of calcining 1-2h, obtains B
Material；
(3) will A material, B mechanical mass mix after be added in ethanol solution, at room temperature by the acetic acid solution of chitosan be added dropwise into
After entering, it is warming up to 35-40 DEG C of stirring 1-5h, mixture is placed in flask, Rotary Evaporators vacuum distillation removes solvent, will consolidate
Body material is washed to 120-150 DEG C of drying after neutrality after pouring out.
3. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(1) mass concentration of sodium hydroxide solution is 5-20% in.
4. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(1) oxidant is hydrogen peroxide or sodium hypochlorite in.
5. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(1) mass ratio of the quality of ferric sulfate and tapioca is 1:15-40 in.
6. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(1) mass ratio of Macrogol 6000 and tapioca is 1:20-25 in.
7. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(1) mass concentration of calcium chloride solution is 0.5-2.5% in.
8. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(2) mass concentration of the ethanol solution of melamine is 20-30% in.
9. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
(3) A material in, B material mass ratio be 4-8:1.
10. the preparation method that dyeing and printing sewage as claimed in claim 2 handles porous spheroidal adsorbent, which is characterized in that step
Suddenly the mass concentration of the acetic acid solution of chitosan is 10-15% in (3).
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