CN108821309A - In the method for industrial wastes coproduction ammonium nitrate and hexagonal plate magnesium hydroxide - Google Patents
In the method for industrial wastes coproduction ammonium nitrate and hexagonal plate magnesium hydroxide Download PDFInfo
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- CN108821309A CN108821309A CN201811030838.XA CN201811030838A CN108821309A CN 108821309 A CN108821309 A CN 108821309A CN 201811030838 A CN201811030838 A CN 201811030838A CN 108821309 A CN108821309 A CN 108821309A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/18—Nitrates of ammonium
- C01C1/185—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The present invention provides a kind of methods with industrial wastes coproduction ammonium nitrate and hexagonal plate magnesium hydroxide, this method is by designing reasonable processing route, using industrial wastes as raw material, the magnesium hydroxide of the ammonium nitrate and 95% of 95% or more recycling or more, realizing turns waste into wealth, the purpose of contamination-reducing synergistic, production cost can be reduced for manufacturing enterprise, the discharge amount of waste water is greatly reduced in pole, and enterprise is made to more easily reach environmental requirement, and the purpose of energy-saving and emission-reduction is realized for enterprise.At the same time, the ammonium nitrate products and hexagonal plate magnesium hydroxide product morphological rules, good dispersion that coproduction is prepared according to the method for the present invention have good market application prospect.
Description
Technical field
The invention belongs to industrial wastes processing technology fields, it relates in particular to which one kind is with industrial wastes coproduction ammonium nitrate
And the method for hexagonal plate magnesium hydroxide.
Background technique
Chemistry has penetrated into the every aspect of human lives, is related to every field, complex chemical composition is various, Hen Duodou
It is the substance for having pollution to environment, being harmful to the human body, the waste liquid generated in production process, if being discharged into living area, Jiu Huiwei
Human lives are coerced, bring harm to human and environment；And certain production waste liquids have certain economic value, in order to improve resource
Comprehensive utilization ratio, strive for clean manufacturing, certain measure taken before discharging of waste liquid to its purified treatment and recycles benefit
With useful component, the protection to environment and the effective use of resource may be implemented.
For that in the development process of phosphorus ore, can generate various production waste liquids, one of which is useless for domestic enterprise at present
Liquid basic composition is：4mol/L~7mol/L NH4 +, 0.4mol/L~1mol/L Mg2+, 5mol/L~10mol/LNO3 -, and
A small amount of Ca2+、Na+、K+、SO4 2-、PO4 3-、F-、SiO3 2-Etc. other ions.As can be seen that containing a large amount of NH in the waste liquid4 +
And Mg2+If can be recycled, the pollution of waste liquid can be not only reduced, moreover it is possible to improve resource utilization.
A kind of substance of ammonium nitrate smokeless or few cigarette when being from a wealth of sources, low detonation, burning, is widely used, can be with
As fertilizer, analytical reagent, oxidant, insecticide, refrigerant, and can be used for manufacturing laughing gas, pyrotechnics and explosive etc..Ammonium nitrate
Production method has conversion method and two kinds of neutralisation.It is original that conversion method, which is using the by-product four water-calcium nitrate of Phosphate Fertilizer Production process,
Material, is reacted with sal volatile, generates ammonium nitrate and precipitation of calcium carbonate, through filtering, filtrate be processed into ammonium nitrate products or
Return to Phosphate Fertilizer Production system.The neutralization reaction of neutralisation can carry out under normal pressure, pressurization or vacuum condition.Industrially adopt
With it is more be 50%~60% with concentration nitric acid and ammonia carried out under 0.4MPa~0.5MPa pressurized conditions in and obtain
Ammonium nitrate solution, concentration are 80%~87%, are then concentrated to 95%~99% with the method for vacuum evaporation or falling film evaporation, most
It is differently granulated afterwards.
Magnesium hydroxide is at home and abroad increasingly subject to weight as efficient, superior, environmentally friendly novel addition inorganic fire retardants
Depending on having obtained significant progress in inorganic fire retardants field.The multi-functionals such as its fire-retardant, smoke elimination, resistance drop, filling, in polymer
Materials industry is used widely.With being constantly progressive for society, continuous improvement of the people to advance material requirement, magnesium hydroxide is produced
The quality index of product not only rests in initial product purity, also proposed to product form and size distribution higher
It is required that.Mg(OH)2Production technology there are many, the precipitation method are the main methods of present production magnesium hydroxide, and that reports at present is heavy
The method that shallow lake method prepares magnesium hydroxide mainly has direct precipitation method, hydro-thermal reaction method, sluggish precipitation, reversed-phase precipitation, homogeneous
Flow process etc..Due to special appearance and the magnesium hydroxide of even particle size distribution, excellent performance, mesh are shown in its application field
Preceding research contents focus mostly on particle fine and prepare the magnesium hydroxide of special appearance.
Most of ammonium nitrate and the production of magnesium hydroxide are prepared using the above method, therefore, above-mentioned needs
If the waste liquid generated in the phosphorus ore development process of discharge can be recycled, comprehensive utilization ratio, the drop of resource are not only increased
The low harm to environment, and the preparation path of ammonium nitrate and/or magnesium hydroxide is additionally provided, reduce preparation cost.
Summary of the invention
To solve the above-mentioned problems of the prior art, the present invention provides one kind with industrial wastes coproduction ammonium nitrate and
95% or more ammonium nitrate can be recycled by technological design using industrial wastes as raw material for the method for hexagonal plate magnesium hydroxide
And 95% or more magnesium hydroxide, realizing turns waste into wealth, the purpose of contamination-reducing synergistic.
In order to achieve the above object of the invention, present invention employs the following technical solutions：
A method of with industrial wastes coproduction ammonium nitrate and hexagonal plate magnesium hydroxide, including step：
S1, industrial wastes is concentrated by evaporation at 50 DEG C~90 DEG C to crystallisation by cooling after 1h~10h, and filters the first filter of acquisition
Cake and the first filtrate；Wherein, in the industrial wastes, NH4 +Concentration be 4mol/L~7mol/L, Mg2+Concentration be
0.4mol/L~1mol/L, NO3 -Concentration be 5mol/L~10mol/L；
The preparation of S2, ammonium nitrate products, include the following steps：
S21, by first filter cake in prefabricated ammonium nitrate saturated solution, dispensing laundry simultaneously filters, obtain second filter
Cake；
S22, at room temperature by second filter cake according to 1.5:1~2.5:1 mass ratio is dissolved in deionized water, is obtained
Ammonium nitrate solution；Wherein, the mass percent of water is 29%~40% in the ammonium nitrate solution；
S23, the ammonium nitrate solution is concentrated by evaporation at 50 DEG C~90 DEG C fall 15%~35% water after crystallisation by cooling,
And it filters and obtains third filter cake；
S24, the dry third filter cake obtain the ammonium nitrate products；
The preparation of S3, hexagonal plate magnesium hydroxide product, include the following steps：
S31, under stirring conditions, is warming up to 30 DEG C~80 DEG C for first filtrate, then with 1mL/min~
The lye of 2mol/L~14mol/L is added in first filtrate by the charging rate of 20mL/min, and ageing 10min~
60min obtains the first suspension；
S32, filtering first suspension, obtain the 4th filter cake；
After S33, washing the 4th filter cake, it is scattered in hydro-thermal medium, the hydro-thermal reaction at 120 DEG C~200 DEG C
1h~48h obtains the second suspension；
S34, filtering second suspension, obtain the 5th filter cake；
It is dried after S35, washing the 5th filter cake to the hydro-thermal medium without entrainment, obtains the hexagonal plate hydrogen-oxygen
Change magnesium products.
Further, in the step S1, the industrial wastes produces phosphorus concentrate, phosphoric acid from mid low grade phosphate rock
And its production waste liquid generated when salt and/or phosphorus simple substance product.
Further, in the step S33, the hydro-thermal medium is deionized water or concentration no more than 6mol/L's
Sodium hydroxide solution or potassium hydroxide solution.
Further, in the step S23, third filtrate corresponding with the third filter cake is also obtained；Described
Three filtrates are back in the step S21 for replacing the ammonium nitrate saturated solution.
Further, in the step S21, the second filtrate corresponding with second filter cake is also obtained；Described
Two filtrates are back in the step S1 and are evaporated concentration jointly with the industrial wastes.
Further, in the step S32, the 4th filtrate corresponding with the 4th filter cake is also obtained；Described
Four filtrates are back in the step S1 and are evaporated concentration jointly with the industrial wastes.
Further, in the step S34, the 5th filtrate corresponding with the 5th filter cake is also obtained；Described 5th
Filtrate is back in the step S33, the 4th filter cake and the hydro-thermal instead of the part hydro-thermal medium and after washing
Medium mixing carries out hydro-thermal reaction.
Further, in the step S35, also generation is washed after washing the 5th filter cake to the hydro-thermal medium without entrainment
Liquid；The washing lotion is for preparing the hydro-thermal medium.
Further, in the step S24, dry 1h~10h, acquisition at 30 DEG C~80 DEG C by the third filter cake
The ammonium nitrate products；And/or in the step S35, the 5th filter cake after washing is done at 80 DEG C~120 DEG C
Dry 5h~10h obtains the hexagonal plate magnesium hydroxide product.
The present invention is by designing reasonable processing route, using industrial wastes as raw material, the ammonium nitrate of 95% or more recycling with
And 95% or more magnesium hydroxide, realizing turns waste into wealth, the purpose of contamination-reducing synergistic, can for manufacturing enterprise reduce production cost,
The discharge amount of waste water is greatly reduced in pole, and enterprise is made to more easily reach environmental requirement, and the purpose of energy-saving and emission-reduction is realized for enterprise.
The ammonium nitrate products and hexagonal plate magnesium hydroxide product morphological rules, good dispersion that coproduction of the present invention is prepared, have
Good market application prospect.
Detailed description of the invention
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing：
Fig. 1 is the technique of the method according to the present invention with industrial wastes coproduction ammonium nitrate and hexagonal plate magnesium hydroxide
Flow chart；
Fig. 2 is the XRD diagram piece of powdered ammonium nitrate products made from embodiment according to the present invention 1；
Fig. 3 is the local camera photos of powdered ammonium nitrate products made from embodiment according to the present invention 1；
Fig. 4 is the XRD diagram piece of hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 1；
Fig. 5 and Fig. 6 is hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 1 under different multiplying
SEM picture；
Fig. 7 is the XRD diagram piece of needle-shaped ammonium nitrate products made from embodiment according to the present invention 2；
Fig. 8 is the local camera photos of needle-shaped ammonium nitrate products made from embodiment according to the present invention 2；
Fig. 9 and Figure 10 is hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 2 under different multiplying
SEM picture；
Figure 11 is the grain size distribution of hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 2；
Figure 12 is the XRD diagram piece of rodlike ammonium nitrate products made from embodiment according to the present invention 3；
Figure 13 is the local camera photos of rodlike ammonium nitrate products made from embodiment according to the present invention 3；
Figure 14 and Figure 15 is hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 3 under different multiplying
SEM picture；
Figure 16 is the grain size distribution of hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 3；
Figure 17 is the XRD diagram piece of rodlike ammonium nitrate products made from embodiment according to the present invention 4；
Figure 18 is the local camera photos of rodlike ammonium nitrate products made from embodiment according to the present invention 4；
Figure 19 is the XRD diagram piece of hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 4；
Figure 20 and Figure 21 is hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 4 under different multiplying
SEM picture；
Figure 22 is the XRD diagram piece of hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 5；
Figure 23 and Figure 24 is hexagonal plate magnesium hydroxide product made from embodiment according to the present invention 5 under different multiplying
SEM picture.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to which there are many different forms to come in fact
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, providing these implementations
Example is in order to explain the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
Term " first ", " second " etc. herein can be used to describe various substances although will be appreciated that, these
Substance should not be limited by these terms.These terms are only used to distinguish a substance with another substance.
The present invention is based on industrial wastes, especially mid low grade phosphate rock production phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance
The production waste liquid generated when product, proposes one kind using it as raw material, coproduction ammonium nitrate and hexagonal plate magnesium hydroxide
Method.
In above-mentioned industrial wastes, it basic composition is：The NH of 4mol/L~7mol/L4 +, 0.4mol/L~1mol/L
Mg2+, 5mol/L~10mol/L NO3 -；Also, when its be particularly limited as mid low grade phosphate rock production phosphorus concentrate, phosphoric acid and its
When the production waste liquid generated when salt and/or phosphorus simple substance product, wherein also containing a small amount of Ca2+、Na+、K+、SO4 2-、PO4 3-、F-、
SiO3 2-Etc. other ions, still, these foreign ions have no apparent influence for presently disclosed process.
Specifically, refering to fig. 1, this method includes the following steps：
In step sl, industrial wastes is concentrated by evaporation to crystallisation by cooling after 1h~10h at 50 DEG C~90 DEG C, and filters and obtains
Obtain the first filter cake and the first filtrate.
In step s 2, ammonium nitrate products are prepared.
Referring particularly to following step：
S21, by the first filter cake in prefabricated ammonium nitrate saturated solution, dispensing laundry simultaneously filters, obtain the second filter cake and
Second filtrate.
There can be the first filtrate component that part is carried secretly by the first filter cake in second filtrate obtained, but it remains as nitre
The saturated solution of sour ammonium, therefore preferably the second filtrate is back in step S1, merge with industrial wastes be evaporated jointly it is dense
Contracting.
S22, at room temperature by the second filter cake according to 1.5:1~2.5:1 mass ratio is dissolved in deionized water, obtains nitric acid
Ammonium salt solution.
In this way, the mass percent for controlling wherein water is 29%~40% in ammonium nitrate solution obtained.
S23, ammonium nitrate solution is concentrated by evaporation at 50 DEG C~90 DEG C fall 15%~35% water after crystallisation by cooling, and mistake
Filter obtains third filter cake and third filtrate.
Bulk composition is the ammonium nitrate solution being saturated in third filtrate obtained, with nitric acid prefabricated in step S21
Ammonium saturated solution is similar；In this way, prefabricated ammonium nitrate saturated solution is substituted in step S21 it is preferred that returning it to, to
One filter cake carries out dispensing laundry；In this way, the recycling of ammonium nitrate on the one hand can be gradually increased during gradually recycling
Rate also reduces the industrial wastes on the other hand without preparing the ammonium nitrate solution being saturated in addition with the first filter cake of dispensing laundry
Processing cost.In other words, when the process starts for the first time, it is molten to need to prepare a certain amount of ammonium nitrate saturation in advance
Liquid (i.e. above-mentioned ammonium nitrate saturated solution) then may be used to the first filter cake of dispensing laundry, but after the final ammonium nitrate products of output
The third filtrate cycle use that will be generated at this time.
S24, dry third filter cake obtain ammonium nitrate products.
Third filter cake is preferably dried 1h~10h by dry specific method at 30 DEG C~80 DEG C.
In step s3, hexagonal plate magnesium hydroxide product is prepared.
Referring particularly to following step：
S31, under stirring conditions, is warming up to 30 DEG C~80 DEG C for the first filtrate, then with 1mL/min~20mL/min
Charging rate the lye of 2mol/L~14mol/L is added in the first filtrate, be aged 10min~60min, it is outstanding to obtain first
Turbid.
Specifically, first the first filtrate can be placed in reactor, and is warming up to 30 DEG C~80 under stirring conditions
℃；At the same time, the lye for being 2mol/L~14mol/L with deionized water compound concentration, and by its with 1mL/min~
The charging rate of 20mL/min, which is added in the first filtrate for have warmed up completion, carries out synthetic reaction, then by 10min~
The ageing of 60min obtains the first suspension.
S32, the first suspension of filtering, obtain the 4th filter cake and the 4th filtrate.
Bulk composition is the Mg in complete first filtrate of a small amount of unreacted in 4th filtrate obtained2+, it is a large amount of original
Ammonium nitrate and generate the 4th filter cake in magnesium hydroxide when the newly-generated ammonium nitrate of metathesis reaction therefore return it to
It is evaporated concentration in step S1 jointly with industrial wastes, this is for effectively improving NH in the industrial wastes4 +And Mg2+Return
Yield is very crucial.
S33, washing the 4th filter cake after, be scattered in hydro-thermal medium, at 120 DEG C~200 DEG C hydro-thermal reaction 1h~
48h obtains the second suspension.
Specifically, hydro-thermal medium, which can be the lye etc. of water or concentration no more than 6mol/L, can aid in magnesium hydroxide
Realize the substance of dissolving-recrystallization；Also, above-mentioned lye is preferably sodium hydroxide solution or potassium hydroxide solution.
For the washing of the 4th filter cake without the progress of a large amount of water in this step, it is only necessary to slightly wash,
It is preferred that the deionized water using 2~3 times of the 4th filter cake volume is washed 2 times；The washing operation of 4th filter cake is not necessarily to
A large amount of water can also substantially save slurry, further decrease separation costs.
S34, the second suspension of filtering, obtain the 5th filter cake and the 5th filtrate.
Bulk composition is similar to hydro-thermal medium and therefore returns it in step S43, generation in 5th filtrate obtained
For part hydro-thermal medium with washing after the 4th filter cake and hydro-thermal medium mix progress hydro-thermal reaction.
It is dried after S35, the 5th filter cake of washing to the hydro-thermal medium without entrainment, obtains hexagonal plate magnesium hydroxide and produce
Product.
Preferably, will the 5th Washing of Filter Cake to after the hydro-thermal medium without entrainment, by its at 80 DEG C~120 DEG C dry 5h~
10h can be obtained hexagonal plate magnesium hydroxide product.
Also, washing lotion is also generated after the 5th filter cake of washing to the hydro-thermal medium without entrainment, there are still few in this part washing lotion
The effective component for measuring hydro-thermal medium, can be recycled, for preparing hydro-thermal medium.
In this way, the above method of the invention passes through the reasonable processing route of design, using industrial wastes as raw material, recycling
The magnesium hydroxide of 95% or more ammonium nitrate and 95% or more, realizing turns waste into wealth, the purpose of contamination-reducing synergistic, can be production
Enterprise reduces production cost, and pole is greatly reduced the discharge amount of waste water, enterprise is made to more easily reach environmental requirement, is that enterprise is real
The purpose of existing energy-saving and emission-reduction.At the same time, ammonium nitrate products and hexagonal plate magnesium hydroxide that coproduction of the present invention is prepared
Product morphological rules, good dispersion have good market application prospect.
It is worth noting that in the technological design of method of the invention, there is technical issues that following and most
Overcome eventually, obtains the above method of the invention.
1) main component for the industrial wastes that the present invention is based on is ammonium nitrate and magnesium nitrate, but inventor's discovery is direct
Ammonium hydroxide is added thereto or highly basic precipitates magnesium in advance and isolated processing route is unworkable, even if adding into the industrial wastes
Enter 20~30 times of Mg2+It is but generated without any sediment when the ammonium hydroxide of the amount of substance, and it is molten that a large amount of highly basic is added into waste liquid
When liquid, seldom sediment can only be also generated, by carefully analyzing and studying, discovery reason may be a large amount of NH4 +Presence tool
There is OH- buffer function, the ionization of ammonium hydroxide can be inhibited.Based on this, the present invention is based on many experiments to propose in advance through pervaporation
The liquid (i.e. the first filtrate) obtained after concentration-crystallisation by cooling and filter operation then can produce a large amount of precipitating when adding ammonium hydroxide
Object；Therefore the processing route of method proposed by the present invention is finally confirmed as：It initially evaporates concentration-crystallisation by cooling, be obtained by filtration
Then ammonium nitrate ammonium hydroxide is added into the first filtrate and prepares magnesium hydroxide.
2) crystallisation by cooling after being concentrated by evaporation industrial wastes at 50 DEG C~90 DEG C, and it is nitric acid that bulk composition, which is obtained by filtration,
First filter cake of ammonium contains Mg in first filter cake2+、Ca2+、NO3 -Equal impurity, but ammonium nitrate is substance soluble easily in water, no
It can directly be washed with water, therefore select its saturated solution to wash, and in order to improve detersive efficiency, by the be obtained by filtration first filter
Cake is transferred to agitator treating in prefabricated ammonium nitrate saturated solution, to most impurity be removed, then by dissolving, steaming again
Hair concentration, crystallisation by cooling, filter operation further remove a small amount of residual impurity, and the ammonium nitrate products of high-purity are prepared, and
The third filtrate being obtained by filtration can be used for washing the first filter cake since impurity content is less.
3) the present inventor has found during many experiments, and the 4th filter cake contains a small amount of impurity, to be yellowish,
Rather than the white of magnesium hydroxide, no matter being washed with how many deionized water cannot all be washed as white, and thus analyzing its reason can
Can be easy to reunite and carried a small amount of other impurity secretly, therefore need because the obtained magnesium hydroxide surface polarity of atmospheric synthesis is strong
Will to the magnesium hydroxide of atmospheric synthesis carry out hydrothermal modification, by dissolving-recrystallization process obtain surface polarity it is small, it is not easy to reunite,
The magnesium hydroxide of good dispersion, and facts proved that the magnesium hydroxide after hydro-thermal is white, dispersibility is fabulous.
4) ammonium nitrate is stable at normal temperature, but under high temperature and pressure, when sharply heating, all can when by sharp pounding
It explodes.Either solid ammonium nitrate or ammonium nitrate solution all have violent explosivity, and some researches show that containing few
The aqueous ammonium nitrate solution blast temperature that the mass fraction for measuring potassium chloride is 80% is only 220 DEG C.Solid is main in first suspension
For magnesium hydroxide, and liquid is mainly the ammonium nitrate solution of high concentration, it is contemplated that the safety issue of experimental work, it is of the invention
First suspension is not carried out hydrothermal modification directly in the design of process route by inventor, but is first filtered and obtain afterwards
Four filter cakes, then the 4th filter cake is added to be uniformly dispersed in hydro-thermal medium after carry out hydrothermal modification.
It will be illustrated below by specific embodiment of the invention above-mentioned with industrial wastes coproduction ammonium nitrate and hexagonal
The method of flake magnesium hydroxide, but this method is not limited to listed parameter in following embodiments, and following parameters are only the above methods
Specific example.
Embodiment 1
The production for taking Guizhou phosphorus ore factory to generate when producing phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance product is useless
For liquid as industrial wastes raw material, concrete composition is as shown in table 1.
The main composition of 1 industrial wastes of table
Unit：g/L
Referring particularly to following step, come coproduction ammonium nitrate products and hexagonal plate hydroxide by raw material of above-mentioned industrial wastes
Magnesium products.
Firstly, under stirring conditions by above-mentioned industrial wastes in 80 DEG C of evaporation and concentration 8h, crystallisation by cooling obtains after filtering
First filter cake and the first filtrate.
Secondly, preparing ammonium nitrate products as raw material using the first filter cake.
Specifically, the first filter cake 1) under stirring conditions, is added to the prefabricated ammonium nitrate containing trace impurity
It washs and filters in saturated solution, obtain the second filter cake and the second filtrate；It 2) is 2 according to mass ratio by the second filter cake:1 is dissolved in
Ammonium nitrate solution is obtained in ionized water, and the ammonium nitrate solution is warming up to 90 DEG C under stirring conditions and is concentrated by evaporation 30%
Water then forces cooled and filtered with cooling water, obtains third filter cake and third filtrate；3) by third filter cake under the conditions of 50 DEG C
Dry 5h, obtains powdered ammonium nitrate products.
In the present embodiment, the second filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；And third filtrate is back to and substitutes prefabricated ammonium nitrate saturated solution in subsequent cycle.
X-ray diffraction test (hereinafter referred to as XRD) is carried out to the product that this step obtains, and is taken pictures to its apparent form；
Its picture and photo difference are as shown in Figures 2 and 3.Fig. 2 and Fig. 3 confirms that products obtained therefrom is powdered ammonium nitrate products.
It is worth noting that being the ammonium nitrate that will be prepared in the camera photos of the ammonium nitrate products of the present embodiment
Product, which is placed in surface plate, carries out acquisition of taking pictures；Also, in order to more clearly from show its apparent form, by its integral photograph
Part carries out screenshot and shows.Camera photos in following each embodiments are similarly.
Finally, preparing hexagonal plate magnesium hydroxide product as raw material using the first filtrate.
Specifically, the first filtrate 1) is warming up to 60 DEG C under stirring conditions, then will with the speed of 5mL/min
The ammonium hydroxide of 14mol/L, which is added in the first filtrate, carries out synthetic reaction, is aged 15min, obtains the first suspension；2) filter this
One suspension obtains the 4th filter cake and the 4th filtrate；3) after washing the 4th filter cake, it is added to the sodium hydroxide solution of 4mol/L
In, it is stirring evenly and then adding into autoclave, hydro-thermal reaction 3h under conditions of 300r/min, 150 DEG C, it is outstanding to obtain second
Turbid；4) the second suspension is filtered, the 5th filter cake and the 5th filtrate are obtained；5) the 5th filter cake is washed to hydro-thermal Jie without entrainment
After matter, dry 10h, screening obtain the hexagonal plate hydrogen of good dispersion, morphological rules, even particle size distribution under the conditions of 105 DEG C
Magnesium oxide product.
In the present embodiment, the 4th filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；5th filtrate, which is back in subsequent cycle, replaces part sodium hydroxide solution as the 4th after hydro-thermal medium, with washing
Filter cake and sodium hydroxide solution mixing carry out hydro-thermal reaction；Also, will wash the washing lotion that generates after the 5th filter cake be back to it is subsequent
For preparing hydro-thermal medium in cyclic process.
The product obtained to this step successively carries out the sem test under XRD test and different multiplying (hereinafter referred to as
SEM)；Its picture is respectively as shown in Fig. 4 and Fig. 5, Fig. 6.Fig. 4~Fig. 6 confirms products obtained therefrom for hexagonal plate magnesium hydroxide production
Product.
Embodiment 2
The production for taking Guizhou phosphorus ore factory to generate when producing phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance product is useless
For liquid as industrial wastes raw material, concrete composition is as shown in table 2.
The main composition of 2 industrial wastes of table
Unit：g/L
Referring particularly to following step, come coproduction ammonium nitrate products and hexagonal plate hydroxide by raw material of above-mentioned industrial wastes
Magnesium products.
Firstly, under stirring conditions by above-mentioned industrial wastes in 60 DEG C of evaporation and concentration 10h, crystallisation by cooling obtains after filtering
Obtain the first filter cake and the first filtrate.
Secondly, preparing ammonium nitrate products as raw material using the first filter cake.
Specifically, the first filter cake 1) under stirring conditions, is added to the prefabricated ammonium nitrate containing trace impurity
It washs and filters in saturated solution, obtain the second filter cake and the second filtrate；It 2) is 2 according to mass ratio by the second filter cake:1 is dissolved in
Ammonium nitrate solution is obtained in ionized water, and the ammonium nitrate solution is warming up to 80 DEG C under stirring conditions and is concentrated by evaporation 20%
Water then forces cooled and filtered with cooling water under conditions of gentle agitation, obtains third filter cake and third filtrate；3) by
Three filter cakes dry 5h under the conditions of 50 DEG C, obtains needle-shaped ammonium nitrate products.
In the present embodiment, the second filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；And third filtrate is back to and substitutes prefabricated ammonium nitrate saturated solution in subsequent cycle.
XRD test is carried out to the product that this step obtains, and is taken pictures to its apparent form；Its picture and photo are respectively as schemed
Shown in 7 and Fig. 8.Fig. 7 and Fig. 8 confirms that products obtained therefrom is needle-shaped ammonium nitrate products.
Finally, preparing hexagonal plate magnesium hydroxide product as raw material using the first filtrate.
Specifically, the first filtrate 1) is warming up to 60 DEG C under stirring conditions, then will with the speed of 2.5mL/min
The ammonium hydroxide of 14mol/L, which is added in the first filtrate, carries out synthetic reaction, is aged 15min, obtains the first suspension；2) filter this
One suspension obtains the 4th filter cake and the 4th filtrate；3) after washing the 4th filter cake, it is added to the sodium hydroxide solution of 4mol/L
In, it is stirring evenly and then adding into autoclave, which is placed in insulating box, water under conditions of 160 DEG C
Thermal response 20h obtains the second suspension；4) the second suspension is filtered, the 5th filter cake and the 5th filtrate are obtained；5) the 5th filter cake passes through
After washing to the hydro-thermal medium without entrainment, dry 10h, screening obtain good dispersion, morphological rules, granularity under the conditions of 105 DEG C
The hexagonal plate magnesium hydroxide product being evenly distributed.
In the present embodiment, the 4th filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；5th filtrate, which is back in subsequent cycle, replaces part sodium hydroxide solution as the 4th after hydro-thermal medium, with washing
Filter cake and sodium hydroxide solution mixing carry out hydro-thermal reaction；Also, will wash the washing lotion that generates after the 5th filter cake be back to it is subsequent
For preparing hydro-thermal medium in cyclic process.
The SEM test under different multiplying is carried out to the product that this step obtains；Its picture difference is as shown in Figure 9 and Figure 10.
Fig. 9, Figure 10 confirm that products obtained therefrom is hexagonal plate magnesium hydroxide product.
At the same time, the particle diameter distribution of the hexagonal plate magnesium hydroxide product obtained to the present embodiment is tested,
Middle D10It is 1.849 μm, D50It is 3.405 μm, D90It is 6.436 μm, as shown in figure 11.As can be seen that the hydrogen-oxygen that the present embodiment obtains
It is uniform to change magnesium particle diameter distribution, granularity is 3.4 μm.
Embodiment 3
The production for taking Guizhou phosphorus ore factory to generate when producing phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance product is useless
For liquid as industrial wastes raw material, concrete composition is as shown in table 3.
The main composition of 3 industrial wastes of table
Unit：g/L
Referring particularly to following step, come coproduction ammonium nitrate products and hexagonal plate hydroxide by raw material of above-mentioned industrial wastes
Magnesium products.
Firstly, under stirring conditions by above-mentioned industrial wastes in 60 DEG C of evaporation and concentration 10h, crystallisation by cooling obtains after filtering
Obtain the first filter cake and the first filtrate.
Secondly, preparing ammonium nitrate products as raw material using the first filter cake.
Specifically, the first filter cake 1) under stirring conditions, is added to the prefabricated ammonium nitrate containing trace impurity
It washs and filters in saturated solution, obtain the second filter cake and the second filtrate；It 2) is 2 according to mass ratio by the second filter cake:1 is dissolved in
Ammonium nitrate solution is obtained in ionized water, and the ammonium nitrate solution is warming up to 70 DEG C under stirring conditions and is concentrated by evaporation 15%
Water forces cooled and filtered with cooling water, obtains third filter cake and third filtrate；3) third filter cake is dry under the conditions of 50 DEG C
5h obtains rodlike ammonium nitrate products.
In the present embodiment, the second filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；And third filtrate is back to and substitutes prefabricated ammonium nitrate saturated solution in subsequent cycle.
XRD test is carried out to the product that this step obtains, and is taken pictures to its apparent form；Its picture and photo are respectively as schemed
Shown in 12 and Figure 13.Figure 12 and Figure 13 confirms that products obtained therefrom is rodlike ammonium nitrate products.
Finally, preparing hexagonal plate magnesium hydroxide product as raw material using the first filtrate.
Specifically, the first filtrate 1) is warming up to 60 DEG C under stirring conditions, then will with the speed of 5mL/min
The ammonium hydroxide of 4mol/L, which is added in the first filtrate, carries out synthetic reaction, is aged 15min, obtains the first suspension；2) filter this
One suspension obtains the 4th filter cake and the 4th filtrate；3) after washing the 4th filter cake, it is added to the sodium hydroxide solution of 4mol/L
In, it is stirring evenly and then adding into autoclave, which is placed in insulating box, water under conditions of 160 DEG C
Thermal response 20h obtains the second suspension；4) the second suspension is filtered, the 5th filter cake and the 5th filtrate are obtained；5) the 5th filter cake passes through
After washing to the hydro-thermal medium without entrainment, dry 10h, screening obtain good dispersion, morphological rules, granularity under the conditions of 110 DEG C
The hexagonal plate magnesium hydroxide product being evenly distributed.
In the present embodiment, the 4th filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；5th filtrate, which is back in subsequent cycle, replaces part sodium hydroxide solution as the 4th after hydro-thermal medium, with washing
Filter cake and sodium hydroxide solution mixing carry out hydro-thermal reaction；Also, will wash the washing lotion that generates after the 5th filter cake be back to it is subsequent
For preparing hydro-thermal medium in cyclic process.
The SEM test under different multiplying is carried out to the product that this step obtains；Its picture difference is as shown in Figure 14 and Figure 15.
Figure 14, Figure 15 confirm that products obtained therefrom is hexagonal plate magnesium hydroxide product.
At the same time, the particle diameter distribution of the hexagonal plate magnesium hydroxide product obtained to the present embodiment is tested,
In, D10It is 0.145 μm, D50It is 1.795 μm, D90It is 4.767 μm, as shown in figure 16.As can be seen that the hydrogen that the present embodiment obtains
Magnesia particle diameter distribution is uniform, and granularity is 1.8 μm.
Embodiment 4
The production for taking Guizhou phosphorus ore factory to generate when producing phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance product is useless
For liquid as industrial wastes raw material, concrete composition is as shown in table 4.
The main composition of 4 industrial wastes of table
Unit：g/L
Referring particularly to following step, come coproduction ammonium nitrate products and hexagonal plate hydroxide by raw material of above-mentioned industrial wastes
Magnesium products.
Firstly, under stirring conditions by above-mentioned industrial wastes in 90 DEG C of evaporation and concentration 8h, crystallisation by cooling obtains after filtering
First filter cake and the first filtrate.
Secondly, preparing ammonium nitrate products as raw material using the first filter cake.
Specifically, the first filter cake 1) under stirring conditions, is added to the prefabricated ammonium nitrate containing trace impurity
It washs and filters in saturated solution, obtain the second filter cake and the second filtrate；It 2) is 2 according to mass ratio by the second filter cake:1 is dissolved in
Ammonium nitrate solution is obtained in ionized water, and the ammonium nitrate solution is warming up to 50 DEG C under stirring conditions and is concentrated by evaporation 15%
Water filters after natural cooling, obtains third filter cake and third filtrate；3) third filter cake is dried to 5h under the conditions of 50 DEG C, is obtained
Rodlike ammonium nitrate products.
In the present embodiment, the second filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；And third filtrate is back to and substitutes prefabricated ammonium nitrate saturated solution in subsequent cycle.
XRD test is carried out to the product that this step obtains, and is taken pictures to its apparent form；Its picture and photo are respectively as schemed
Shown in 17 and Figure 18.Figure 17 and Figure 18 confirms that products obtained therefrom is rodlike ammonium nitrate products.
Finally, preparing hexagonal plate magnesium hydroxide product as raw material using the first filtrate.
Specifically, the first filtrate 1) is warming up to 60 DEG C under stirring conditions, then will with the speed of 15mL/min
The ammonium hydroxide of 4mol/L, which is added in the first filtrate, carries out synthetic reaction, is aged 15min, obtains the first suspension；2) filter this
One suspension obtains the 4th filter cake and the 4th filtrate；3) it after washing the 4th filter cake, is add to deionized water, after mixing evenly
It is added in autoclave, which is placed in insulating box, hydro-thermal reaction 40h under conditions of 180 DEG C is obtained
Second suspension；4) the second suspension is filtered, the 5th filter cake and the 5th filtrate are obtained；5) the 5th filter cake is washed to without entrainment
After hydro-thermal medium, dry 10h, screening obtain good dispersion, morphological rules, the hexagonal of even particle size distribution under the conditions of 105 DEG C
Hydroxide flake magnesium products.
In the present embodiment, the 4th filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make.
SEM under XRD test and different multiplying test is successively carried out to the product that this step obtains；Its picture is respectively as schemed
19 and Figure 20, Figure 21 shown in.Figure 19~Figure 21 confirms that products obtained therefrom is hexagonal plate magnesium hydroxide product.
Embodiment 5
The production for taking Guizhou phosphorus ore factory to generate when producing phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance product is useless
For liquid as industrial wastes raw material, concrete composition is as shown in table 5.
The main composition of 5 industrial wastes of table
Unit：g/L
Referring particularly to following step, come coproduction ammonium nitrate products and hexagonal plate hydroxide by raw material of above-mentioned industrial wastes
Magnesium products.
Firstly, under stirring conditions by above-mentioned industrial wastes in 90 DEG C of evaporation and concentration 8h, crystallisation by cooling obtains after filtering
First filter cake and the first filtrate.
Secondly, preparing ammonium nitrate products as raw material using the first filter cake.
Specifically, the first filter cake 1) under stirring conditions, is added to the prefabricated ammonium nitrate containing trace impurity
It washs and filters in saturated solution, obtain the second filter cake and the second filtrate；It 2) is 2 according to mass ratio by the second filter cake:1 is dissolved in
Ammonium nitrate solution is obtained in ionized water, and the ammonium nitrate solution is warming up to 50 DEG C under stirring conditions and is concentrated by evaporation 15%
Water filters after natural cooling, obtains third filter cake and third filtrate；3) third filter cake is dried to 5h under the conditions of 50 DEG C, is obtained
Rodlike ammonium nitrate products.
In the present embodiment, the second filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；And third filtrate is back to and substitutes prefabricated ammonium nitrate saturated solution in subsequent cycle.
Finally, preparing hexagonal plate magnesium hydroxide product as raw material using the first filtrate.
Specifically, the first filtrate 1) is warming up to 60 DEG C under stirring conditions, then will with the speed of 15mL/min
The ammonium hydroxide of 4mol/L, which is added in the first filtrate, carries out synthetic reaction, is aged 15min, obtains the first suspension；2) filter this
One suspension obtains the 4th filter cake and the 4th filtrate；3) it after washing the 4th filter cake, is add to deionized water, after mixing evenly
It is added in autoclave, which is placed in insulating box, hydro-thermal reaction 20h under conditions of 180 DEG C is obtained
Second suspension；4) the second suspension is filtered, the 5th filter cake and the 5th filtrate are obtained；5) the 5th filter cake is washed to without entrainment
After hydro-thermal medium, dry 10h, screening obtain good dispersion, morphological rules, the hexagonal of even particle size distribution under the conditions of 110 DEG C
Hydroxide flake magnesium products.
In the present embodiment, the 4th filtrate is back in subsequent cycle to merge with industrial wastes and carries out evaporation and concentration behaviour
Make；5th filtrate, which is back in subsequent cycle, replaces part sodium hydroxide solution as the 4th after hydro-thermal medium, with washing
Filter cake and sodium hydroxide solution mixing carry out hydro-thermal reaction；Also, will wash the washing lotion that generates after the 5th filter cake be back to it is subsequent
For preparing hydro-thermal medium in cyclic process.
SEM under XRD test and different multiplying test is successively carried out to the product that this step obtains；Its picture is respectively as schemed
22 and Figure 23, Figure 24 shown in.Figure 22~Figure 24 confirms that products obtained therefrom is hexagonal plate magnesium hydroxide product.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (9)
1. a kind of method with industrial wastes coproduction ammonium nitrate and hexagonal plate magnesium hydroxide, which is characterized in that including step：
S1, industrial wastes is concentrated by evaporation to crystallisation by cooling after 1h~10h at 50 DEG C~90 DEG C, and filter obtain the first filter cake and
First filtrate；Wherein, in the industrial wastes, NH4 +Concentration be 4mol/L~7mol/L, Mg2+Concentration be 0.4mol/L
~1mol/L, NO3 -Concentration be 5mol/L~10mol/L；
The preparation of S2, ammonium nitrate products, include the following steps：
S21, by first filter cake in prefabricated ammonium nitrate saturated solution, dispensing laundry simultaneously filters, obtain the second filter cake；
S22, at room temperature by second filter cake according to 1.5:1~2.5:1 mass ratio is dissolved in deionized water, obtains nitric acid
Ammonium salt solution；Wherein, the mass percent of water is 29%~40% in the ammonium nitrate solution；
S23, the ammonium nitrate solution is concentrated by evaporation at 50 DEG C~90 DEG C fall 15%~35% water after crystallisation by cooling, and mistake
Filter obtains third filter cake；
S24, the dry third filter cake obtain the ammonium nitrate products；
The preparation of S3, hexagonal plate magnesium hydroxide product, include the following steps：
S31, under stirring conditions, is warming up to 30 DEG C~80 DEG C for first filtrate, then with 1mL/min~20mL/min
Charging rate the lye of 2mol/L~14mol/L is added in first filtrate, be aged 10min~60min, obtain the
One suspension；
S32, filtering first suspension, obtain the 4th filter cake；
After S33, washing the 4th filter cake, be scattered in hydro-thermal medium, at 120 DEG C~200 DEG C hydro-thermal reaction 1h~
48h obtains the second suspension；
S34, filtering second suspension, obtain the 5th filter cake；
It is dried after S35, washing the 5th filter cake to the hydro-thermal medium without entrainment, obtains the hexagonal plate magnesium hydroxide
Product.
2. the method according to claim 1, wherein in the step S1, during the industrial wastes derives from
The production waste liquid generated when low-grade phosphate ore production phosphorus concentrate, phosphoric acid and its salt and/or phosphorus simple substance product.
3. the method according to claim 1, wherein the hydro-thermal medium is deionization in the step S33
Water or concentration are no more than the sodium hydroxide solution or potassium hydroxide solution of 6mol/L.
4. method according to claim 1 to 3, which is characterized in that in the step S23, also obtain and described the
The corresponding third filtrate of three filter cakes；The third filtrate is back in the step S21 for replacing the ammonium nitrate to be saturated
Solution.
5. method according to claim 1 to 3, which is characterized in that in the step S21, also obtain and described the
Corresponding second filtrate of two filter cakes；Second filtrate is back in the step S1 is steamed jointly with the industrial wastes
Hair concentration.
6. method according to claim 1 to 3, which is characterized in that in the step S32, also obtain and described the
Corresponding 4th filtrate of four filter cakes；4th filtrate is back in the step S1 is steamed jointly with the industrial wastes
Hair concentration.
7. method according to claim 1 to 3, which is characterized in that in the step S34, also obtain and described the
Corresponding 5th filtrate of five filter cakes；5th filtrate is back in the step S33, instead of the part hydro-thermal medium with
The 4th filter cake and hydro-thermal medium mixing after washing carry out hydro-thermal reaction.
8. method according to claim 1 to 3, which is characterized in that in the step S35, wash the 5th filter
Washing lotion is also generated after cake to the hydro-thermal medium without entrainment；The washing lotion is for preparing the hydro-thermal medium.
9. method according to claim 1 to 3, which is characterized in that in the step S24, by the third filter cake
Dry 1h~10h, obtains the ammonium nitrate products at 30 DEG C~80 DEG C；And/or in the step S35, after washing
5th filter cake dry 5h~10h at 80 DEG C~120 DEG C, obtains the hexagonal plate magnesium hydroxide product.
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