A kind of preparation method of aluminium ore flocculating agent for red mud precipitation
Technical field
The present invention relates to aluminium ore red-mud settlement technical fields, and in particular to a kind of preparation side of aluminium ore flocculating agent for red mud precipitation
Method.
Background technique
Aluminum oxide industry is the basic raw material industry of national economy, plays important work to the development of Chinese industrial economy
With the yield of China's aluminium oxide ranks first in the world.Alumina-producing method is all made of alkaline process at present, and red mud slurry is bauxite
The suspension of red mud and sodium aluminate solution composition after alkali soluble goes out.Slurries make red mud and aluminium by sedimentation or filtering after dilution
Acid sodium solution separates, and then produces aluminium oxide by sodium aluminate solution.The sedimentation separation of red mud is to influence aluminium oxide production capacity, product
One of matter and the key link of benefit.In order to strengthen the sedimentation separation of red mud, alumina producing factory and correlative study institute are done
A large amount of work.Purpose is to improve the sinking speed of red mud, the density of improvement subsider overflowing liquid quality and underflow, to mention
The production efficiency of high equipment and production cost is reduced, and adding flocculant is to generally use at present and effective method, is opened
The hot subject that hair novel flocculant technology is always studied both at home and abroad, state produce the raw material of aluminium oxide mainly with intractable one
Based on diaspore, there is very big difference with external boehmite and gibbsite.
In production technology, foreign countries use Bayer process, and China also uses intensified-sintered and mixed connection etc. in addition to Bayer process
Method.Red mud ingredient and foreign countries are widely different, so that polymer inlet flocculant is selective to domestic red-mud separation.In recent years
Nail (unit of length) section, cyanogen spy and the France for coming the U.S. like that the external major company such as gloomy is directed to China's bauxite feature and does a lot of work, and develop
Some novel flocculants, but external manufacturer holds its effective component and technology of preparing in close confidence, and expensive, because
This, exploitation has independent intellectual property right, is suitable for the new and effective flocculant of China's bauxite red mud sedimentation separation to China
The development of aluminum oxide industry is significant, and flocculant used in red-mud separation is mainly the polyacrylate of anionic at present
Or the hydrolysate of polyacrylamide, dosage form are mainly the hydrosol, dry powder and low concentration reversed-phase emulsion, water-soluble gluey or powdery
Flocculant hygroscopicity is strong, and effective active composition is caused to reduce, and causes additive amount big, and flocculating effect is unstable, and synthetic technology is single,
Low concentration reversed-phase emulsion haves the shortcomings that molecular weight is low, stability is poor again, and using effect is also undesirable.
Summary of the invention
In order to overcome the deficiencies of the prior art, the invention discloses a kind of preparation methods of aluminium ore flocculating agent for red mud precipitation.
To achieve the above object the present invention adopts the following technical scheme:
The invention proposes a kind of preparation methods of aluminium ore flocculating agent for red mud precipitation, include the following steps:
S1, stock, 90~180 parts of acrylic acid, 100~150 parts of ammonium hydroxide, 80~140 parts of deionized water, acrylamide 8~
60 parts, 2~6 parts of ammonium sulfate, 5~50 parts of sodium acrylate, 1~8 part of β-monomethyl itaconate, disodium ethylene diamine tetraacetate 0.15~
1.5 parts, 0.05~0.3 part of sodium hypophosphite, 0.25~1.0 part of di-isopropyl peroxydicarbonate, 110~150 parts of cycloalkane,
8~12 parts of grease, 5~50 parts of hydroxamic acid agent, 15~20 parts of nonionic surface active agent;
15~30 parts of deionized water and 0.05~0.3 part of sodium hypophosphite are passed through stirring and dissolving and obtained by S2, liquid processed
Sodium hypophosphite solution for standby takes remaining deionized water to be added in reaction kettle, by the third of 90~180 parts during stirring
Olefin(e) acid slowly pours into reaction kettle, and reaction kettle is mounted in constant temperature water box, keeps temperature of reaction kettle in 10~30 DEG C of conditions
After 100~150 parts of ammonium hydroxide of lower addition, acrylic acid inside reaction kettle and ammonium hydroxide mix, by 8~60 parts of acrylamide, 2~
6 parts of ammonium sulfate, 5~50 parts of sodium acrylate, 1~8 part of β-monomethyl itaconate, 0.15~1.5 part of ethylenediamine tetrem
Acid disodium and 0.25~1.0 part of di-isopropyl peroxydicarbonate are implanted sequentially in reaction kettle, continue that constant temperature is kept to continue to stir
It mixes, until stirring is completely dissolved, is configured to polymerized emulsion and continues to employ, by measure 110~150 parts of cycloalkane, 8~12 parts
Grease is sequentially added in agitator tank and is stirred, and is stirred evenly to internal solution, and oil liquid is obtained;
Oil liquid obtained in S2 is slowly injected into configuration in S2 and completed in the reaction kettle of polymerized emulsion, together by S3, mixing
When be stirred, then ortho phosphorous acid sodium solution obtained in S2 is injected into temperature in 25~70 DEG C of reaction kettle, to temperature
When stopping rising, keep the temperature of reaction kettle at 45~70 DEG C by constant temperature water box, after the reaction time for keeping 1.5~4h,
Temperature is improved to 80~95 DEG C, 5~50 parts of hydroxamic acid agent is slowly added in reaction kettle;
S4, discharging, will be anti-by constant temperature water box after reacting 3~7h by the reaction kettle that hydroxamic acid agent reaction is added in S3
It answers kettle internal temperature to be down to 40~55 DEG C, then 15~20 parts of nonionic surface active agent is slowly added in reaction kettle, together
When be stirred, aluminium ore flocculating agent for red mud precipitation lotion needed for being obtained after being mixed after 0.5~1h to be mixed.
Preferably, the hydroxamic acid agent is hydroxylamine hydrochloride.
Preferably, the nonionic surface active agent is sorbitan fatty acid ester, glyceryl stearate, fatty alcohol
One of aliphatic ester and polyoxyethylene fatty acid ester or a variety of mixing.
Preferably, the aluminium ore flocculating agent for red mud precipitation lotion, which is evaporated under reduced pressure, is made solid content up to 50~55% flocculants
Lotion finished product.
Compared with prior art, the beneficial effects of the present invention are: the present invention is mixed using monomer polymerization lotion and modified emulsion
Stirring is closed, mutually method is slowly dropped into salt water relative to traditional oil, saves a large amount of reaction time, improve production efficiency, and mixed
Dissolved after conjunction it is uniform, final products be free of organic solvent, while using β-monomethyl itaconate both effectively prevent polymerization Shi Yikang
Sour single chain transfer, and be conducive to aluminium ore red mud for the effective carboxyl functional group of long-chain introducing and tangle, play " frame
The effect of bridge " achievees the purpose that separation, improves the sinking speed of red mud, safer to environment and operator, hence it is evident that improves
The clarity of supernatant, reduces waste, and product sedimentation separation effect in the application of aluminium ore red mud improves particularly evident.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.The specific embodiments described herein are merely illustrative of the present invention, is not used to limit
The present invention.
Embodiment 1
S1,90 parts of acrylic acid, 100 parts of ammonium hydroxide, 80 parts of deionized water, 25 parts of acrylamide, 2 parts of ammonium sulfate, acrylic acid are taken
10 parts of sodium, 1 part of β-monomethyl itaconate, disodium ethylene diamine tetraacetate 0.15,0.05 part of sodium hypophosphite, dicetyl peroxydicarbonate two
0.25 part of isopropyl ester, 110 parts of cycloalkane, 8 parts of grease, 5 parts of hydroxamic acid agent, 15 parts of nonionic surface active agent;
The sodium hypophosphite of 15 parts of deionized water and 0.05 part is obtained ortho phosphorous acid by stirring and dissolving by S2, liquid processed
Sodium solution is spare, takes remaining deionized water to be added in reaction kettle, slowly falls 90 parts of acrylic acid during stirring
Entering in reaction kettle, reaction kettle is mounted in constant temperature water box, and keep temperature of reaction kettle that 100 parts of ammonium hydroxide are added under the conditions of 10 DEG C,
After acrylic acid inside reaction kettle and ammonium hydroxide mix, by 25 parts of acrylamide, 2 parts of ammonium sulfate, 10 parts of sodium acrylate,
1 part of β-monomethyl itaconate, 0.15 part of disodium ethylene diamine tetraacetate and 0.25 part of di-isopropyl peroxydicarbonate according to
In secondary injection reaction kettle, continues that constant temperature is kept to continue to stir, until stirring is completely dissolved, is configured to polymerized emulsion and continues to employ, will count
Measured 110 parts of cycloalkane, 8 parts of grease are sequentially added in agitator tank and are stirred, and are stirred evenly to internal solution, are obtained
Oil liquid;
Oil liquid obtained in S2 is slowly injected into configuration in S2 and completed in the reaction kettle of polymerized emulsion, together by S3, mixing
When be stirred, then ortho phosphorous acid sodium solution obtained in S2 is injected into temperature in 25 DEG C of reaction kettle, stopped to temperature
When rising, by constant temperature water box keep reaction kettle temperature at 45 DEG C, after being kept for the reaction time of 1.5h, by temperature improve to
80 DEG C, 5 parts of hydroxamic acid agent is slowly added in reaction kettle;
The reaction kettle of hydroxamic acid agent reaction will be added in S4, discharging in S3, after reacting 3h, will be reacted by constant temperature water box
Kettle internal temperature is down to 40 DEG C, then 15 parts of nonionic surface active agent are slowly added in reaction kettle, is stirred simultaneously, to
Aluminium ore flocculating agent for red mud precipitation lotion needed for being obtained after being mixed after stirring 0.5h.
Embodiment 2
S1, stock, 140 parts of acrylic acid, 120 parts of ammonium hydroxide, 120 parts of deionized water, 40 parts of acrylamide, 4 parts of ammonium sulfate, third
30 parts of olefin(e) acid sodium, 6 parts of β-monomethyl itaconate, 1 part of disodium ethylene diamine tetraacetate, 0.2 part of sodium hypophosphite, dicetyl peroxydicarbonate
0.5 part of diisopropyl ester, 140 parts of cycloalkane, 10 parts of grease, 30 parts of hydroxamic acid agent, 18 parts of nonionic surface active agent;
The sodium hypophosphite of 20 parts of deionized water and 0.2 part is obtained sodium hypophosphite by stirring and dissolving by S2, liquid processed
Solution for standby takes remaining deionized water to be added in reaction kettle, slowly pours into 140 parts of acrylic acid during stirring
In reaction kettle, reaction kettle is mounted in constant temperature water box, keeps temperature of reaction kettle that 120 parts of ammonium hydroxide are added at 20 °C, when
After acrylic acid and ammonium hydroxide inside reaction kettle mix, by 40 parts of acrylamide, 4 parts of ammonium sulfate, 30 parts of sodium acrylate, 6
β-the monomethyl itaconate of part, 1 part and 0.5 part of disodium ethylene diamine tetraacetate of di-isopropyl peroxydicarbonate are implanted sequentially instead
It answers in kettle, continues that constant temperature is kept to continue to stir, until stirring is completely dissolved, is configured to polymerized emulsion and continues to employ, 140 will measured
The cycloalkane, 10 parts of grease of part are sequentially added in agitator tank and are stirred, and are stirred evenly to internal solution, and oil liquid is obtained;
Oil liquid obtained in S2 is slowly injected into configuration in S2 and completed in the reaction kettle of polymerized emulsion, together by S3, mixing
When be stirred, then ortho phosphorous acid sodium solution obtained in S2 is injected into temperature in 50 DEG C of reaction kettle, stopped to temperature
When rising, keeps the temperature of reaction kettle at 55 DEG C by constant temperature water box, after being kept for the reaction time of 3h, temperature is improved to 90
DEG C, 30 parts of hydroxamic acid agent is slowly added in reaction kettle;
The reaction kettle of hydroxamic acid agent reaction will be added in S4, discharging in S3, after reacting 5h, will be reacted by constant temperature water box
Kettle internal temperature is down to 50 DEG C, then 18 parts of nonionic surface active agent is slowly added in reaction kettle, is stirred simultaneously,
Aluminium ore flocculating agent for red mud precipitation lotion needed for being obtained after being mixed after 0.8h to be mixed.
Embodiment 3
S1, stock, 180 parts of acrylic acid, 150 parts of ammonium hydroxide, 140 parts of deionized water, 60 parts of acrylamide, 6 parts of ammonium sulfate, third
50 parts of olefin(e) acid sodium, 8 parts of β-monomethyl itaconate, 1.5 parts of disodium ethylene diamine tetraacetate, 0.3 part of sodium hypophosphite, two carbon of peroxidating
1.0 parts of sour diisopropyl ester, 150 parts of cycloalkane, 12 parts of grease, 50 parts of hydroxamic acid agent, 20 parts of nonionic surface active agent;
The sodium hypophosphite of 30 parts of deionized water and 0.3 part is obtained sodium hypophosphite by stirring and dissolving by S2, liquid processed
Solution for standby takes remaining deionized water to be added in reaction kettle, slowly pours into 180 parts of acrylic acid during stirring
In reaction kettle, reaction kettle is mounted in constant temperature water box, keeps temperature of reaction kettle that 150 parts of ammonium hydroxide are added under the conditions of 30 DEG C, when
After acrylic acid and ammonium hydroxide inside reaction kettle mix, by 60 parts of acrylamide, 6 parts of ammonium sulfate, 50 parts of sodium acrylate, 8
β-the monomethyl itaconate, 1.5 parts of disodium ethylene diamine tetraacetate and 1.0 parts of di-isopropyl peroxydicarbonate of part are successively infused
Enter in reaction kettle, continues that constant temperature is kept to continue to stir, until stirring is completely dissolved, is configured to polymerized emulsion and continues to employ, will measure
150 parts of cycloalkane, 12 parts of grease sequentially add in agitator tank and be stirred, stirred evenly to internal solution, obtain oil
Liquid;
Oil liquid obtained in S2 is slowly injected into configuration in S2 and completed in the reaction kettle of polymerized emulsion, together by S3, mixing
When be stirred, then ortho phosphorous acid sodium solution obtained in S2 is injected into temperature in 70 DEG C of reaction kettle, stopped to temperature
When rising, keeps the temperature of reaction kettle at 70 DEG C by constant temperature water box, after being kept for the reaction time of 4h, temperature is improved to 95
DEG C, 50 parts are slowly added to hydroxamic acid agent in reaction kettle;
The reaction kettle of hydroxamic acid agent reaction will be added in S4, discharging in S3, after reacting 7h, will be reacted by constant temperature water box
Kettle internal temperature is down to 55 DEG C, then 20 parts of nonionic surface active agent is slowly added in reaction kettle, is stirred simultaneously,
Aluminium ore flocculating agent for red mud precipitation lotion needed for being obtained after being mixed after 1h to be mixed.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.