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 field, and in particular to a kind of preparation side of aluminium ore flocculating agent for red mud precipitation
Method.
Background technology
Aluminum oxide industry is the basic raw material industry of national economy, and the development to Chinese industrial economy plays important work
With the yield of China's aluminium oxide ranks first in the world.At present alumina-producing method adopts alkaline process, and red mud slurry is bauxite
The suspension that red mud is constituted with sodium aluminate solution Jing after alkali soluble goes out.Serosity makes red mud and aluminum after dilution by sedimentation or filtration
Acid sodium solution is separated, and then produces aluminium oxide by sodium aluminate solution.The settlement separate of red mud is to affect aluminium oxide production capacity, product
One of key link of matter and benefit.In order to strengthen the settlement separate of red mud, alumina producing factory and correlational study institute, do
Substantial amounts of work.Purpose is to improve the sedimentation velocity of red mud, improves the density of subsider overflowing liquid quality and underflow, to carry
The production efficiency and reduction production cost of high equipment, and it is generally to adopt at present and effective method to add flocculant, is opened
The hot subject that novel flocculant technology is always studied both at home and abroad is sent out, the raw material of state's production aluminium oxide is mainly with intractable one
Based on diaspore, there is very big difference with external boehmite and gibbsite.
In production technology, foreign countries adopt Bayer process, and China also uses intensified-sintered and series-parallel connection etc. in addition to Bayer process
Method.Red mud composition is widely different with foreign countries, so that polymer inlet flocculant is selective to the red-mud separation of the country.In recent years
Come the nail (unit of length) section in the U.S., cyanogen is special and love Lignum Rhamnellae major company of foreign countries of France does a lot of work for Chinese bauxite feature, develop
Some novel flocculants, but external manufacturer holds in close confidence to its effective ingredient and technology of preparing, and also it is expensive, because
This, exploitation has independent intellectual property right, is suitable for the settlement separate new and effective flocculant of China's bauxite red mud to China
The development of aluminum oxide industry is significant, and the flocculant that current red-mud separation is used is mainly the polyacrylate of anionic
Or the hydrolyzate of polyacrylamide, its dosage form is mainly the hydrosol, dry powder and low concentration reversed-phase emulsion, water-soluble gluey or powdery
Flocculant hygroscopicity is strong, causes effective active composition to reduce, and causes addition 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.
The content of the invention
To overcome the deficiencies in the prior art, the invention discloses a kind of preparation method of aluminium ore flocculating agent for red mud precipitation.
For achieving the above object the present invention is adopted the following technical scheme that:
The present invention proposes a kind of preparation method of aluminium ore flocculating agent for red mud precipitation, comprises the steps:
S1, get the raw materials ready, 90~180 parts of acrylic acid, 100~150 parts of ammonia, 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, disodiumedetate 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 surfactant;
S2, liquid processed, 15~30 parts of deionized water and 0.05~0.3 part of sodium hypophosphite are obtained by stirring and dissolving
Sodium hypophosphite solution for standby, takes remaining deionized water and adds in reactor, by the third of 90~180 parts during stirring
Olefin(e) acid is lentamente poured in reactor, and reactor is arranged in constant temperature water box, keeps temperature of reaction kettle in 10~30 DEG C of conditions
100~150 parts of ammonia of lower addition, after the acrylic acid inside reactor and ammonia are mixed, 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 reactor, continue to keep constant temperature to continue to stir
Mix, 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 treats that internal solution stirs, and obtains fluid;
S3, mixing, are slowly injected into obtained fluid in S2 configuration in S2 and complete in the reactor of polymerized emulsion, together
When be stirred, obtained ortho phosphorous acid sodium solution in S2 is being injected into into temperature in 25~70 DEG C of reactor, treat temperature
When stopping rising, the temperature of reactor is kept at 45~70 DEG C by constant temperature water box, after being kept for the response time of 1.5~4h,
Temperature is improved to 80~95 DEG C, 5~50 parts of hydroxamic acid agent is slowly added in reactor;
S4, discharging, will add the reactor of hydroxamic acid agent reaction in S3, after 3~7h of reaction, will be anti-by constant temperature water box
Answer kettle internal temperature to be down to 40~55 DEG C, then 15~20 parts of nonionic surfactant is slowly added in reactor, together
When be stirred, aluminium ore flocculating agent for red mud precipitation emulsion needed for obtaining after mixing after 0.5~1h to be mixed.
Preferably, the hydroxamic acid agent is oxammonium hydrochloride..
Preferably, the nonionic surfactant is sorbitan fatty acid ester, glyceryl stearate, fatty alcohol
One or more mixing in fatty acid ester and polyoxyethylene fatty acid ester.
Preferably, aluminium ore flocculating agent for red mud precipitation emulsion Jing vacuum distillation is obtained solid content up to 50~55% flocculant
Emulsion finished product.
Preferably, the reactor is provided with temperature sensor with constant water bath box.
Compared with prior art, the invention has the beneficial effects as follows:The present invention is mixed using monomer polymerized emulsion and modified emulsion
Stirring is closed, relative to traditional oil phase and saline method is slowly dropped into, save a large amount of response time, improve production efficiency, and also it is mixed
Dissolve homogeneous after conjunction, final products do not contain organic solvent, while clothing health when both effectively having prevented from being polymerized using β-monomethyl itaconate
Sour single chain transfer, and be conducive to aluminium ore red mud to tangle for the effective carboxyl functional group of long-chain introducing, play " frame
The effect of bridge " reaches detached purpose, improves the sedimentation velocity of red mud, safer to environment and operator, hence it is evident that to improve
The clarity of supernatant, reduces and wastes, and product settlement separate effect in aluminium ore red mud application improves particularly evident.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, to this
Invention is further elaborated.Specific embodiment described herein only to explain the present invention, is not used to limit
The present invention.
Embodiment 1
S1, take 90 parts of acrylic acid, 100 parts of ammonia, 80 parts of deionized water, 25 parts of acrylamide, 2 parts of ammonium sulfate, acrylic acid
10 parts of sodium, 1 part of β-monomethyl itaconate, disodiumedetate 0.15,0.05 part of sodium hypophosphite, peroxy dicarbonate 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 surfactant;
S2, liquid processed, ortho phosphorous acid is obtained by 15 parts of deionized water and 0.05 part of sodium hypophosphite by stirring and dissolving
Sodium solution is standby, takes remaining deionized water and adds in reactor, lentamente falls 90 parts of acrylic acid during stirring
In entering reactor, reactor is arranged in constant temperature water box, keeps temperature of reaction kettle that 100 parts of ammonia are added under the conditions of 10 DEG C,
After acrylic acid inside reactor is mixed with ammonia, 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 disodiumedetate and 0.25 part of di-isopropyl peroxydicarbonate according to
In secondary injection reactor, continue to keep constant temperature 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 treat that internal solution stirs, and are obtained
Fluid;
S3, mixing, are slowly injected into obtained fluid in S2 configuration in S2 and complete in the reactor of polymerized emulsion, together
When be stirred, obtained ortho phosphorous acid sodium solution in S2 is being injected into into temperature in 25 DEG C of reactor, treat that temperature stops
During rising, by constant temperature water box keep reactor temperature at 45 DEG C, keep 1.5h response time after, by temperature improve to
80 DEG C, 5 parts of hydroxamic acid agent is slowly added in reactor;
S4, discharging, will add the reactor of hydroxamic acid agent reaction, after reaction 3h, will react by constant temperature water box in S3
Kettle internal temperature is down to 40 DEG C, then by nonionic surfactant 15 parts be slowly added in reactor, while being stirred, treat
Aluminium ore flocculating agent for red mud precipitation emulsion needed for obtaining after mixing after stirring 0.5.
Embodiment 2
S1, get the raw materials ready, 140 parts of acrylic acid, 120 parts of ammonia, 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 disodiumedetate, 0.2 part of sodium hypophosphite, peroxy dicarbonate
0.5 part of diisopropyl ester, 140 parts of cycloalkane, 10 parts of grease, 30 parts of hydroxamic acid agent, 18 parts of nonionic surfactant;
S2, liquid processed, sodium hypophosphite is obtained by 20 parts of deionized water and 0.2 part of sodium hypophosphite by stirring and dissolving
Solution for standby, takes remaining deionized water and adds in reactor, lentamente pours 140 parts of acrylic acid into during stirring
In reactor, reactor is arranged in constant temperature water box, keeps temperature of reaction kettle that 120 parts of ammonia are added under the conditions of 20 DEG C, when
After acrylic acid inside reactor and ammonia mixing, by 40 parts of acrylamide, 4 parts of ammonium sulfate, 30 parts of sodium acrylate, 6
β-the monomethyl itaconate of part, the di-isopropyl peroxydicarbonate of 1 part and 0.5 part of disodiumedetate are implanted sequentially instead
In answering kettle, continue to keep constant temperature to continue to stir, until stirring is completely dissolved, is configured to polymerized emulsion and continues to employ, by measure 140
The cycloalkane of part, 10 parts of grease are sequentially added in agitator tank and are stirred, and treat that internal solution stirs, and obtain fluid;
S3, mixing, are slowly injected into obtained fluid in S2 configuration in S2 and complete in the reactor of polymerized emulsion, together
When be stirred, obtained ortho phosphorous acid sodium solution in S2 is being injected into into temperature in 50 DEG C of reactor, treat that temperature stops
During rising, keep the temperature of reactor at 55 DEG C by constant temperature water box, after being kept for the response time of 3h, temperature is improved to 90
DEG C, 30 parts of hydroxamic acid agent is slowly added in reactor;
S4, discharging, will add the reactor of hydroxamic acid agent reaction, after reaction 5h, will react by constant temperature water box in S3
Kettle internal temperature is down to 50 DEG C, then 18 parts of nonionic surfactant is slowly added in reactor, while be stirred,
Aluminium ore flocculating agent for red mud precipitation emulsion needed for obtaining after mixing after 0.8h to be mixed.
Embodiment 3
S1, get the raw materials ready, 180 parts of acrylic acid, 150 parts of ammonia, 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 disodiumedetate, 0.3 part of sodium hypophosphite, the carbon of peroxidating two
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 surfactant;
S2, liquid processed, sodium hypophosphite is obtained by 30 parts of deionized water and 0.3 part of sodium hypophosphite by stirring and dissolving
Solution for standby, takes remaining deionized water and adds in reactor, lentamente pours 180 parts of acrylic acid into during stirring
In reactor, reactor is arranged in constant temperature water box, keeps temperature of reaction kettle that 150 parts of ammonia are added under the conditions of 30 DEG C, when
After acrylic acid inside reactor and ammonia mixing, by 60 parts of acrylamide, 6 parts of ammonium sulfate, 50 parts of sodium acrylate, 8
Part β-monomethyl itaconate, 1.5 parts of disodiumedetate and 1.0 parts of di-isopropyl peroxydicarbonate note successively
In entering reactor, continue to keep constant temperature to continue to stir, until stirring is completely dissolved, is configured to polymerized emulsion and continues to employ, will measure
150 parts cycloalkane, 12 parts of grease sequentially add in agitator tank and be stirred, treat that internal solution stirs, obtain oil
Liquid;
S3, mixing, are slowly injected into obtained fluid in S2 configuration in S2 and complete in the reactor of polymerized emulsion, together
When be stirred, obtained ortho phosphorous acid sodium solution in S2 is being injected into into temperature in 70 DEG C of reactor, treat that temperature stops
During rising, keep the temperature of reactor at 70 DEG C by constant temperature water box, after being kept for the response time of 4h, temperature is improved to 95
DEG C, 50 parts are slowly added to hydroxamic acid agent in reactor;
S4, discharging, will add the reactor of hydroxamic acid agent reaction, after reaction 7h, will react by constant temperature water box in S3
Kettle internal temperature is down to 55 DEG C, then 20 parts of nonionic surfactant is slowly added in reactor, while be stirred,
Aluminium ore flocculating agent for red mud precipitation emulsion needed for obtaining after mixing after 1h to be mixed.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.