CN109809419A - A method of preparing poly silicate aluminium ferric flocculating agent - Google Patents
A method of preparing poly silicate aluminium ferric flocculating agent Download PDFInfo
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Abstract
The invention discloses a kind of methods for preparing polymeric aluminium ferrum silicate flocculant, the flocculant using industrial solid castoffs such as gangue, flyash, red muds as raw material, by raw material preparation, sinter leaching, water quenching, crude product washing separation, inorganic acid adjust, alkali cleaning and etc. preparation produce.Present invention reduces costs, have saved resource, realize recycling for activator, efficiently avoid the pollution of environment, and process flow is simple, and low energy consumption, and equipment etching problem is simple, are conducive to industrialization promotion.
Description
Technical field
The present invention relates to the solid waste resource recoveries such as gangue, flyash, red mud, and field, more particularly to preparation to be utilized to gather
The method for closing silicate aluminium ferric flocculating agent.
Background technique
In recent years, as the fast development of China's economic society, city and discharged volume of industrial waste water are consequently increased, and I
The water resource of state is very short, and this requires carry out effectively purified treatment and recycling to the waste water of discharge.
Polymeric aluminium ferrum silicate (PSAF) is a kind of novel water-soluble macromolecule electrolyte.It is mainly used for purifying drinking water,
Can also be used in water supply special water quality processing, except cadmium, fluorine removal, radioactive contamination eliminating, except oil slick etc..It is also used at industrial wastewater
Reason, such as dyeing waste water, casting, papermaking, medicine, in terms of be also widely used.It sewage treatment field for
The processing of sewage has the effect of getting instant result, and is current sewage treatment drug very salable.Polymeric aluminium ferrum silicate have from
Sub- degree is high, it is soluble easily in water it is (completely soluble in entire pH range, and do not influenced by low water temperature), not at gel, hydrolysis
The features such as stability is good is a kind of more satisfactory sewage-treating agent.
SiO in gangue, flyash and red mud2、Al2O3、Fe2O3Etc. chemical components, be the master for preparing polymeric aluminium ferrum silicate
Want raw material.And gangue, flyash and red mud discharge for a long time as solid waste, not only cause the waste of resource, but also
A large amount of soils are also occupied, dual destruction is caused to ecology and environment.Therefore, solid to solids such as gangue, flyash and red muds
Body waste carries out effectively resource utilization, prepares effluent purifier, has not only saved cost, but also for economizing on resources,
Improve environment, raising economic and social benefit is of great immediate significance and long-range strategic importance.
Summary of the invention
The present invention provides a kind of methods for preparing polymeric aluminium ferrum silicate flocculant, it is therefore an objective to gangue, flyash and
The industrial solid castoffs such as red mud carry out resource utilization, prepare the polymeric aluminium ferrum silicate flocculant of high added value, save
Resource reduces costs, and improves environment.
The purpose of the present invention is being implemented by following technical solution, however the present invention can come in different forms in fact
It applies, and should not be construed as being limited to embodiment described in this paper.On the contrary, these embodiments are provided, so that this
Invention is thorough and complete to those skilled in the art, and will fully communicate the scope of the present invention.
Unless otherwise defined, all technical and scientific terms used herein have such as the technical field of the invention
The normally understood identical meanings of those of ordinary skill institute.Term used in description herein is specific for describing
Embodiment, rather than be limited.As singular used in this specification and the appended claims
" one ", "one", " described " etc. also include plural form, unless context is clearly indicated otherwise.
On the one hand, the present invention provides a kind of preparation methods of polymeric aluminium ferrum silicate flocculant, it is characterised in that: is with coal
One of spoil, flyash, red mud or it is a variety of prepare poly silicate aluminium ferric flocculating agent for raw material, steps are as follows for specific method:
(1) one of gangue, flyash, red mud or a variety of ball mills that pass through are crushed to 100 mesh or more as mixing original
Material, wherein the ratio of Si/Al/Fe is 5~30/20~50/10~40 in mixed raw material；
(2) mixed raw material in step (1) is uniformly mixed with activator and is prepared into raw material, the activator is ammonium sulfate or chlorine
Change the mixture of ammonium or both, and activator and the mass ratio of mixed raw material are (5~10): 1；
(3) raw material in step (2) are roasted to 1~3h, 0.25~0.3MPa of reaction pressure under conditions of 500~750 DEG C,
Clinker and tail gas are obtained, the tail gas enters process below after heat exchange, and the hot gas obtained after heat exchange is used for
The concentration crystallization step of solution below；
(4) clinker in step (3) is transferred in the water of equal quality and carries out water quenching, obtain particle size at 10~100 μm
Crude product is added to the water of 3 times of volumes after the crude product to be carried out to wet-milling, 2h is sufficiently stirred at 90 DEG C, is then separated by solid-liquid separation
Obtain filtrate A and filter residue B；
(5) hydrogen peroxide that concentration is 30% is added into filtrate A, then passes to the tail gas in step (3) after heat exchange, instead
1h is stirred at 40 DEG C after answering, liquor C and filter cake D are obtained after being separated by solid-liquid separation, as step after the concentrated crystallization of liquor C
Suddenly the activator in (2) is recycled；
(6) after being sufficiently mixed calcium aluminate and filter cake D, inorganic acid is added and is stirred to react 4h, reaction knot under the conditions of 60~80 DEG C
2h is stood after beam, obtains solution E；
(7) it is transferred to and is equipped in the corrosion-resistant autoclave of sodium hydroxide solution after being crushed filter residue B, stirred after being warming up to 130 DEG C
Reaction 4h is mixed, is separated by solid-liquid separation after being cooled to room temperature, obtains solution F；
(8) by solution E with mass ratio (1~1.5): 1 ratio is slowly added into solution F, mixing speed not less than 150 turns/
Minute, 40 DEG C of reaction temperature, solution C passes through after being added adds inorganic acid for adjusting pH value to 3.5~4, obtains after standing 6~12h
Polymeric aluminium ferrum silicate flocculant.
Preferably, tail gas passes through two sections of heat exchange processes in the step (3), obtains 300~350 DEG C after first segment process
High temperature hot gas, 100~150 DEG C of medium temperature hot gas is obtained after second segment process, the high temperature hot gas and medium temperature hot gas are used
In step (5) in the condensing crystallizing process of liquor C.
Preferably, calcium aluminate is the 2~5% of filter cake D mass in the step (6).
Preferably, inorganic acid is added in the step (6) and adjusts pH value to 2.2~2.5.
Preferably, the inorganic acid in the step (6) and step (8) is 3~10% technical hydrochloric acid or 5~15% work
The mixture of industry sulfuric acid or both.
Preferably, the Na in the step (7) in sodium hydroxide solution2SiO in O and filter residue B2Mass ratio control 1:
(0.6~0.8).
On the other hand, the present invention also provides a kind of polymeric aluminium ferrum silicate flocculant, which is by above method system
Standby production.
Compared with prior art, the present invention efficiently utilizes the industrial solid castoffs such as gangue, flyash and red mud
In SiO2、Al2O3、Fe2O3Chemical component prepares polymeric aluminium ferrum silicate flocculant, reduces costs, has saved resource, effectively
Ground avoids the pollution of environment.In addition, process flow of the invention is simple, low energy consumption, and equipment etching problem is simple, is conducive to produce
Industryization is promoted.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Embodiment 1
Gangue, flyash and red mud are mixed using the ratio of 1:1:1.5 as mixed raw material, wherein Si/Al/ in mixed raw material
The ratio of Fe is 30/40/30, can be containing other components such as Ca, Mg, Na, K, Ti in mixed raw material, this cannot be used for limiting this
The protection scope of invention.
The above-mentioned mixed raw material ball mill grinding to 100 mesh of 1000g or more is taken, is uniformly mixed with activator and is prepared into raw material, institute
Stating activator is ammonium chloride, and activator and the mass ratio of mixed raw material are 7:1；The raw material being prepared into are transferred in roaster
It is roasted at 650 DEG C, reaction pressure 0.3MPa, obtains clinker and tail gas after roasting 2h；Tail gas passes through two sections of heat exchange works
Sequence is cooling, obtains 300~350 DEG C of high temperature hot gas after first segment process, obtains in 100~150 DEG C after second segment process
Warm gas, the high temperature hot gas and medium temperature the hot gas concentration crystallization step of solution later；Clinker is transferred to 1.5L's
Water quenching is carried out in water, obtains particle size in 10~100 μm of crude products, and crude product carries out to the water that 4.5L is added to after wet-milling, 90 DEG C
Under 2h is sufficiently stirred, then be separated by solid-liquid separation obtain filtrate A and filter residue B；The dioxygen that 100mL concentration is 30% is added into filtrate A
Water then passes to the tail gas after heat exchange, stirs 1h at 40 DEG C after reaction, obtains after being separated by solid-liquid separation containing chlorination
The liquor C of ammonium and filter cake D containing ferro-aluminum hydroxide, wherein liquor C carries out condensing crystallizing by the hot gas after heat exchange and obtains
It is recycled to ammonium chloride and as activator；After 25g calcium aluminate and filter cake D are sufficiently mixed, 5% technical hydrochloric acid is added simultaneously
PH value is adjusted to 2.2~2.5,4h is stirred to react under the conditions of 60~80 DEG C, stands 2h after reaction, is obtained containing polymerization chlorine
Change the solution E of ferro-aluminum；Filter residue B is transferred to after broken be equipped with the sodium hydroxide solution that 6L concentration is 25% corrosion-resistant high pressure it is anti-
It answers in kettle, is stirred to react 4h after being warming up to 130 DEG C, be separated by solid-liquid separation after being cooled to room temperature, obtain the solution F containing sodium metasilicate；It presses
Solution E is slowly added into solution F by the ratio of mass ratio 1:1, and 180 revs/min of mixing speed, 40 DEG C of reaction temperature, solution C
The Nacl acid for adjusting pH value of addition 5% obtains filemot polymeric aluminium ferrum silicate after standing 12h to 3.5~4 after addition
Flocculant.
Embodiment 2
The mixed raw material ball mill grinding to 100 mesh in 1000g embodiment 1 or more is taken, is uniformly mixed with activator and is prepared into raw material,
The activator is ammonium sulfate, and activator and the mass ratio of mixed raw material are 8:1；The raw material being prepared into are transferred to roaster
In roasted at 650 DEG C, reaction pressure 0.3MPa, roast 2h after obtain clinker and tail gas；Tail gas passes through two sections of heat exchanges
Process is cooling, obtains 300~350 DEG C of high temperature hot gas after first segment process, obtains 100~150 DEG C after second segment process
The concentration crystallization step of medium temperature hot gas, the high temperature hot gas and medium temperature hot gas solution later；Clinker is transferred to 1.5L
Water in carry out water quenching, obtain particle size in 10~100 μm of crude products, crude product carry out to the water for being added to 4.5L after wet-milling, 90
2h is sufficiently stirred at DEG C, is then separated by solid-liquid separation and obtains filtrate A and filter residue B；The dioxygen that 100mL concentration is 30% is added into filtrate A
Water then passes to the tail gas after heat exchange, stirs 1h at 40 DEG C after reaction, obtains after being separated by solid-liquid separation containing sulfuric acid
The liquor C of ammonium and filter cake D containing ferro-aluminum hydroxide, wherein liquor C carries out condensing crystallizing by the hot gas after heat exchange and obtains
It is recycled to ammonium sulfate and as activator；After 25g calcium aluminate and filter cake D are sufficiently mixed, 10% industrial sulphuric acid is added simultaneously
PH value is adjusted to 2.2~2.5,4h is stirred to react under the conditions of 60~80 DEG C, stands 2h after reaction, obtain containing polymerised sulphur
The solution E of sour ferro-aluminum；Filter residue B is transferred to after broken be equipped with the sodium hydroxide solution that 6L concentration is 25% corrosion-resistant high pressure it is anti-
It answers in kettle, is stirred to react 4h after being warming up to 130 DEG C, be separated by solid-liquid separation after being cooled to room temperature, obtain the solution F containing sodium metasilicate；It presses
Solution E is slowly added into solution F by the ratio of mass ratio 1:1, and 180 revs/min of mixing speed, 40 DEG C of reaction temperature, solution C
The industrial sulphuric acid of addition 10% adjusts pH value to 3.5~4 after addition, obtains filemot polymeric aluminium ferrum silicate after standing 12h
Flocculant.
Embodiment 3
5% technical hydrochloric acid and 10% industrial sulphuric acid are mixed to get inorganic acid with 1:1 ratio；Take the mixing in 1000g embodiment 1 former
Expect ball mill grinding to 100 mesh or more, be uniformly mixed with activator and be prepared into raw material, the activator is the chlorination of mass ratio 1:1
Ammonium and ammonium sulfate mixture, and activator and the mass ratio of mixed raw material are 8:1；The raw material being prepared into are transferred in roaster
It is roasted at 650 DEG C, reaction pressure 0.3MPa, obtains clinker and tail gas after roasting 2h；Tail gas passes through two sections of heat exchange works
Sequence is cooling, obtains 300~350 DEG C of high temperature hot gas after first segment process, obtains in 100~150 DEG C after second segment process
Warm gas, the high temperature hot gas and medium temperature the hot gas concentration crystallization step of solution later；Clinker is transferred to 1.5L's
Water quenching is carried out in water, obtains particle size in 10~100 μm of crude products, and crude product carries out to the water that 4.5L is added to after wet-milling, 90 DEG C
Under 2h is sufficiently stirred, then be separated by solid-liquid separation obtain filtrate A and filter residue B；The dioxygen that 100mL concentration is 30% is added into filtrate A
Water then passes to the tail gas after heat exchange, stirs 1h at 40 DEG C after reaction, obtains after being separated by solid-liquid separation containing chlorination
Ammonium, the liquor C of ammonium sulfate and the filter cake D containing ferro-aluminum hydroxide, wherein liquor C is concentrated by the hot gas after heat exchange
Crystallization obtains ammonium chloride and ammonium sulfate and is recycled as activator；After 25g calcium aluminate and filter cake D are sufficiently mixed, it is added
Inorganic acid simultaneously adjusts pH value to 2.2~2.5, is stirred to react 4h under the conditions of 60~80 DEG C, stands 2h after reaction, obtains molten
Liquid E；It is transferred to after filter residue B is crushed in the corrosion-resistant autoclave for being equipped with the sodium hydroxide solution that 6L concentration is 25%, heating
It is stirred to react 4h after to 130 DEG C, is separated by solid-liquid separation after being cooled to room temperature, the solution F containing sodium metasilicate is obtained；1:1's in mass ratio
Solution E is slowly added into solution F by ratio, and 180 revs/min of mixing speed, 40 DEG C of reaction temperature, after solution C is added
Inorganic acid for adjusting pH value is added to 3.5~4, obtains filemot polymeric aluminium ferrum silicate flocculant after standing 12h.
Claims (7)
1. a kind of preparation method of polymeric aluminium ferrum silicate flocculant, it is characterised in that: be in gangue, flyash, red mud
One or more to prepare poly silicate aluminium ferric flocculating agent for raw material, steps are as follows for specific method:
(1) one of gangue, flyash, red mud or a variety of ball mills that pass through are crushed to 100 mesh or more as mixing original
Material, wherein the ratio of Si/Al/Fe is 5~30/20~50/10~40 in mixed raw material；
(2) mixed raw material in step (1) is uniformly mixed with activator and is prepared into raw material, the activator is ammonium sulfate or chlorine
Change the mixture of ammonium or both, and activator and the mass ratio of mixed raw material are (5~10): 1；
(3) raw material in step (2) are roasted to 1~3h, 0.25~0.3MPa of reaction pressure under conditions of 500~750 DEG C,
Clinker and tail gas are obtained, the tail gas enters process below after heat exchange, and the hot gas obtained after heat exchange is used for
The concentration crystallization step of solution below；
(4) clinker in step (3) is transferred in the water of equal quality and carries out water quenching, obtain particle size at 10~100 μm
Crude product is added to the water of 3 times of volumes after the crude product to be carried out to wet-milling, 2h is sufficiently stirred at 90 DEG C, is then separated by solid-liquid separation
To filtrate A and filter residue B；
(5) hydrogen peroxide that concentration is 30% is added into filtrate A, then passes to the tail gas in step (3) after heat exchange, instead
1h is stirred at 40 DEG C after answering, liquor C and filter cake D are obtained after being separated by solid-liquid separation, as step after the concentrated crystallization of liquor C
Suddenly the activator in (2) is recycled；
(6) after being sufficiently mixed calcium aluminate and filter cake D, inorganic acid is added and is stirred to react 4h, reaction knot under the conditions of 60~80 DEG C
2h is stood after beam, obtains solution E；
(7) it is transferred in the corrosion-resistant autoclave for being equipped with sodium hydroxide solution after being crushed filter residue B, after being warming up to 130 DEG C
It is stirred to react 4h, is separated by solid-liquid separation after being cooled to room temperature, solution F is obtained；
(8) by solution E with mass ratio (1~1.5): 1 ratio is slowly added into solution F, mixing speed not less than 150 turns/
Minute, 40 DEG C of reaction temperature, solution C passes through after being added adds inorganic acid for adjusting pH value to 3.5~4, obtains after standing 6~12h
Polymeric aluminium ferrum silicate flocculant.
2. a kind of preparation method of polymeric aluminium ferrum silicate flocculant according to claim 1, it is characterised in that: the step
(3) tail gas passes through two sections of heat exchange processes in, obtains 300~350 DEG C of high temperature hot gas, second segment process after first segment process
The concentration knot of 100~150 DEG C of medium temperature hot gas, the high temperature hot gas and medium temperature hot gas for liquor C in step (5) is obtained afterwards
In brilliant process.
3. a kind of preparation method of polymeric aluminium ferrum silicate flocculant according to claim 1, it is characterised in that: the step
(6) calcium aluminate is the 2~5% of filter cake D mass in, and after inorganic acid is added, and adjusts pH value to 2.2~2.5.
4. a kind of preparation method of polymeric aluminium ferrum silicate flocculant according to claim 1, it is characterised in that: the step
(6) inorganic acid is added in and adjusts pH value to 2.2~2.5.
5. a kind of preparation method of polymeric aluminium ferrum silicate flocculant according to claim 1, it is characterised in that: in the step
Suddenly the inorganic acid in (6) and step (8) is the mixture of 3~10% technical hydrochloric acid or 5~15% industrial sulphuric acid or both.
6. a kind of preparation method of polymeric aluminium ferrum silicate flocculant according to claim 1, it is characterised in that: the step
(7) Na in sodium hydroxide solution2SiO in O and filter residue B2Mass ratio control in 1:(0.6~0.8).
7. a kind of polymeric aluminium ferrum silicate flocculant, it is characterised in that: use method described in any one of claims 1-6 preparation life
It produces.
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Cited By (1)
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| CN110627099A (en) * | 2019-11-06 | 2019-12-31 | 山东聚杰环保科技有限公司 | Method for preparing high-purity aluminum sulfate and co-producing poly-silicon ferric aluminum sulfate by using waste catalyst |
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| CN110627099A (en) * | 2019-11-06 | 2019-12-31 | 山东聚杰环保科技有限公司 | Method for preparing high-purity aluminum sulfate and co-producing poly-silicon ferric aluminum sulfate by using waste catalyst |
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| CN109809419B (en) | 2022-06-14 |
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