CN103819592B - A kind of preparation method of flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud - Google Patents
A kind of preparation method of flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud Download PDFInfo
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- CN103819592B CN103819592B CN201410078336.XA CN201410078336A CN103819592B CN 103819592 B CN103819592 B CN 103819592B CN 201410078336 A CN201410078336 A CN 201410078336A CN 103819592 B CN103819592 B CN 103819592B
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Abstract
The present invention relates to a kind of preparation method of flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud.The preparation of flocculation agent take high molecular weight polyacrylamide as raw material, adopts hydroxamic acidization and is hydrolyzed the one pot process technique of simultaneously carrying out, prepared hydroxamic acid and carboxyl-content respectively up to 39.8% and 47.6% flocculation agent, and this synthesis step is simple.The flocculation agent of synthesis has good effect to the sedimentation of red mud in China now low-grade high silicon high iron diaspore type bauxite Bayer process production, overcome the industry of existing alumina producing to need to add the difficult problem of multiple flocculation agent for red-mud settlement and separation, reduce cost, meet industrial requirements.
Description
Technical field
The present invention relates to a kind of can the preparation method of flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud.
Background technology
Along with the exhaustion of China's bauxite resource, the grade of the difficult diaspore type bauxite that alumina producer uses is more and more lower, the ratio of its siliceous mineral and iron-bearing mineral increases, and has occurred a large amount of high silicon high iron diaspore type bauxite, has caused the generation of high silicon high iron type Bayer process red mud.But, the commodity flocculation agent of the above-mentioned red mud of existing sedimentation generally only containing carboxyl or Hydroxamic acid, although or simultaneously containing above-mentioned group, carboxyl and Hydroxamic acid content all too low, can not effective settlement separate high silicon high iron type Bayer process red mud.
In addition, nineteen ninety Lewellyn etc. uses the flocculation agent of polyacrylamide (PAM) synthesizing oxygen-containing oxime acid groups in aqueous, Hydroxamic acid content is the highest only reaches 27%(LewellynME for it, SpitzerDP.Preparationofmodifiedacrylamidepolymers.US:490 2751 [P] .1990-02-20), Hydroxamic acid content not only in flocculation agent is not high, and only high to the iron level Bayer process red mud of this flocculation agent has good settlement separate effect.Lu Hong plum in 2003 (Lu Hongmei. a kind of flocculation agent preparation method [J] of effective settlement separate high silicon high iron type Bayer process red mud. Mineral Engineering, 2003 (4): 35-38) in water solution system, prepare flocculation agent, but in this flocculation agent, hydroxamic acid content is the highest only reaches 28%.Wang Shanshan in 2009 etc. (Wang Shanshan. the development [J] of water-soluble hydroxamic acid polymer flocculation agent. chemical engineering abstracts, 2009,03:29-30) to be raw material with polyacrylamide in Syntheses in water system with oxammonium hydrochloride be properties-correcting agent synthesis hydroxamic acid flocculation agent, but the Hydroxamic acid content in this flocculation agent is unknown, and this flocculation agent only can for the treatment of the oily(waste)water in oilfield sewage station.
Mostly be intended to improve its Hydroxamic acid content about the oxygen oximate modified-reaction of polyacrylamide in above-mentioned document, act on iron-bearing mineral, bibliographical information is had no to high silicon high iron type precipitation of red mud in Bayer process separation flocculation agent.
Liu Ming in 2007 waits so long (Liu Mingjiu, Xie Shengli, Hou Niansheng. manufacture method .CN101117262 [P] .2007-07-25 of bayer process red mud flocculating agent) be raw material with polyacrylamide, be hydrolyzed 5 ~ 24 hours in the basic conditions, carry out oxygen oximation reaction with oxammonium hydrochloride afterwards, wherein amide group and azanol mol ratio 0.36 ~ 0.98, temperature of reaction is at 70 ~ 85 DEG C, 3-7 hour, then carries out Mannich reaction, has prepared the amphoteric ionic polyacrylamide of oxygen-containing nitrolic acid group.But be still difficult in this flocculation agent actual application reach the efficient flocculating requirement to high silicon high iron type Bayer process red mud; On the other hand, because red-mud settlement and separation carries out under 95 ~ 100 DEG C of strong alkaline conditions, quaternary ammonium salt cationic group exists with quaternary ammonium hydroxide form under strongly alkaline conditions, and quaternary ammonium hydroxide easily decomposes under 95 ~ 100 DEG C of conditions, lose throwing out (ZhangKunyu, HuHuiping, etal.Thermaldecompositionbehaviourofpolyacrylamidomethyl trimethylammoniumchlorideinredmudseparationprocess [J] .J.Cent.SouthUniv.Technol.2008 (15): 808 ~ 813).
Summary of the invention
The object of the present invention is to provide a kind of hydroxamic acid and carboxyl-content all high and can the preparation method of flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud, this preparation method be simple, and is applicable to suitability for industrialized production.
Technical scheme of the present invention
A preparation method for the flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud, be dissolved in water polyacrylamide, obtains polyacrylamide solution; Under inert gas atmosphere, oxammonium hydrochloride is dissolved in NaOH solution, obtains hydroxylamine hydrochloride solution; Again by above-mentioned polyacrylamide solution and hydroxylamine hydrochloride solution mixing, reaction; In hydroxyamine groups in described oxammonium hydrochloride and polyacrylamide, the mol ratio of amide group is 1.2 ~ 1.5, and the pH in reaction process is 13 ~ 14, and temperature of reaction is 90 ~ 100 DEG C, and the reaction times is 24 ~ 48h.
Under inert gas atmosphere, preferably oxammonium hydrochloride is dissolved in the NaOH solution of equimolar ratio.
The matter average molecular weight of above-mentioned polyacrylamide is preferably 2000 ~ 3,000 ten thousand, and limiting viscosity is preferably 1200 ~ 1750mL/g.
PH in reaction process is preferably by adding the sodium hydroxide solution adjustment that concentration is 20 ~ 40g/L.
React while stirring in reaction process, rotating speed during stirring is preferably 45 ~ 60r/min.
After above-mentioned reaction completes, in reaction system, add dehydrated alcohol further, and close neutral to washings for several times with absolute ethanol washing, after 50 ~ 60 DEG C of vacuum-drying 15 ~ 20h, obtain solid phase prod.
Beneficial effect of the present invention
The present invention has carried out further optimization to the preparation method of prior art and reaction conditions.Under the reaction conditions of the present invention, can increase degree of hydrolysis while control oxygen oximate, prepare hydroxamic acid and carboxyl-content respectively up to 39.8% and 47.6% flocculation agent.This flocculation agent can effective settlement separate high silicon high iron type Bayer process red mud.Concrete, when preparing this flocculation agent, take polyacrylamide as raw material, adopt hydroxamic acidization and be hydrolyzed the one pot process technique of simultaneously carrying out, prepare hydroxamic acid and all high flocculation agent of carboxyl-content, this synthesis step is simple, and have good effect to the settlement separate of red mud in China now low-grade high silicon high iron diaspore type bauxite Bayer process production, overcome alumina producing industry to need to add the difficult problem of multiple flocculation agent for red-mud settlement and separation, reduce cost, meet industrial requirements.
Embodiment
Following examples are intended to that the invention will be further described, instead of limitation of the invention.
Embodiment 1
The flocculation agent of oxygen-containing nitrolic acid and carboxyl is simultaneously prepared under differential responses pH condition
1) high molecular weight polyacrylamide (matter average molecular weight be 2000 ~ 3,000 ten thousand, limiting viscosity be 1200 ~ 1750mL/g) being taken 3.505g after the dry 12h of 50 DEG C of vacuum drying ovens joins in 250mL tri-neck round-bottomed flask, add 100mL distilled water, make high molecular weight polyacrylamide dissolve completely at 40 DEG C of water-baths, 45 ~ 60r/min mechanical stirring 3h;
2) in a nitrogen atmosphere, oxammonium hydrochloride is dissolved in the sodium hydroxide solution of equimolar ratio, slowly be added drop-wise in the polyacrylamide solution of step 1) gained with dropping funnel by it, the mol ratio controlling amide group in oxammonium hydrochloride and polyacrylamide is 1.2 ~ 1.5;
3) whole reaction process control condition: 45 ~ 60r/min mechanical stirring, regulate reactant aqueous solution system pH to be 13 ~ 14 with the NaOH of 20 ~ 40g/L, temperature of reaction is 90 DEG C, and the reaction times is 48h; ;
4) after having reacted, by dehydrated alcohol reprecipitation reaction product, and close neutral to washings for several times with absolute ethanol washing, and filter cake obtains solid phase prod after 50 ~ 60 DEG C of vacuum-drying 15 ~ 20h.
Embodiment 2
The flocculation agent of oxygen-containing nitrolic acid and carboxyl is simultaneously prepared under differential responses temperature condition
Except reaction process condition is: reaction system pH is 14, temperature of reaction is 90 ~ 100 DEG C, and the reaction times is outside 48h, according to the method that embodiment 1 is same, prepares flocculation agent.
Embodiment 3
The flocculation agent of oxygen-containing nitrolic acid and carboxyl is simultaneously prepared under differential responses time conditions
Except reaction process condition is: reaction system pH is 14, temperature of reaction is 90 DEG C, and the reaction times is outside 24 ~ 48h, according to the method that embodiment 1 is same, prepares flocculation agent.
Comparative example 1
The flocculation agent prepared under low alkalinity condition
Except reaction process condition is: reaction system pH is 3 ~ 8, temperature of reaction is 90 DEG C, and the reaction times is outside 48h, according to the method that embodiment 1 is same, prepares flocculation agent.
Comparative example 2
The flocculation agent prepared under low reaction temperatures condition
Except reaction process condition is: reaction system pH is 14, temperature of reaction is 20 ~ 60 DEG C, and the reaction times continues outside 48h, according to the method that embodiment 1 is same, prepares flocculation agent.
Comparative example 3
Reaction times is compared with the flocculation agent prepared under billet part
Except reaction process condition is: reaction system pH is 14, temperature of reaction is 90 DEG C, and the reaction times continues, outside 5 ~ 15h, according to the method that embodiment 1 is same, to prepare flocculation agent.
Comparative example 4
Adopt the flocculation agent prepared under being first hydrolyzed again oxygen oximate condition
1) high molecular weight polyacrylamide (matter average molecular weight be 2000 ~ 3,000 ten thousand, limiting viscosity be 1200 ~ 1750mL/g) is taken 3.505g after the dry 12h of 50 DEG C of vacuum drying ovens to join in 250mL tri-neck round-bottomed flask, add 100mL distilled water and sodium hydroxide.Wherein the weight ratio of polyacrylamide and sodium hydroxide is 1:0.06 ~ 0.12, at 50 DEG C of hydrolysis reaction 7h;
2) after polyacrylamide cooling, it is slowly added oxammonium hydrochloride by dropping funnel, and in oxammonium hydrochloride and polyacrylamide, the mol ratio of amide group is 1.2 ~ 1.5, by the NaOH adjust ph of 20 ~ 40g/L to 12, is warmed up to 70 DEG C and reacts 7h;
3) after having reacted, by dehydrated alcohol reprecipitation reaction product, and close neutral to washings for several times with absolute ethanol washing, and filter cake obtains solid phase prod after 50 ~ 60 DEG C of vacuum-drying 15 ~ 20h.
The mensuration of Hydroxamic acid, carboxyl and amide group content in product
With the total content of carboxylic acid sodium in conductometric titration measure product and hydroxamic acid sodium anionic group, by the nitrogen content in Kjeldahl determination measure product, be converted into the content of hydroxamic acid sodium and amide group part.Two kinds of methods combining can record the ratio of three kinds of functional groups in product macromolecular chain.
That is: take the product of about 0.1g, be accurate to 0.0001g.Be put into by product in small beaker, adding distil water stirs and makes it dissolve, and dissolves completely rear constant volume to 150mL.With the titration of dilute hydrochloric acid standardized solution under continuous stirring, record specific conductivity adds the change of volume with hydrochloric acid.With hydrochloric acid volume for X-coordinate, be that ordinate zou makes titration curve with specific conductivity, the intersection point finding out two fitting a straight lines is titration end point, is the volume of the hydrochloric acid standard solution of consumption, and the total mole number of hydroxamic acid sodium thus in counting yield and sodium carboxylate groups.In the HPAM flocculation agent of synthesis, the content of Hydroxamic acid, carboxyl, amide group can be calculated by three relational expressions below:
x+y+z=1（1）
The percentage mole number of x, y, z-sodium carboxylate groups, hydroxamic acid sodium group, amide group;
94,109, the molar mass of 71-sodium carboxylate groups, hydroxamic acid sodium group, amide group;
M
1the quality product (g) weighed during-survey specific conductivity;
C
1the concentration (mol/L) of titration hydrochloric acid standard solution used during-survey specific conductivity;
V
1the volume (mL) of the hydrochloric acid standard solution that titration consumes during-survey specific conductivity;
M
2the quality product (g) weighed during-Kjeldahl determination;
C
2the concentration (mol/L) of titration hydrochloric acid standard solution used during-Kjeldahl determination;
V
2the volume (mL) of the hydrochloric acid standard solution that titration consumes during-Kjeldahl determination.
Performance test
Use the flocculation agent prepared in embodiment and comparative example to the settlement separate effect of red mud in certain high silicon high iron diaspore type bauxite bayer process ' s digested slurry domestic.Main containing 20 ~ 25% rhombohedral iron ore, 18 ~ 21% pyrrhosiderites, 34 ~ 40% calcium aluminosilicate hydrates, 8 ~ 10% cancrinites, 2% calcium titanate in red mud.Before separating experiment, diluted by bauxite Bayer dissolved mineral slurry, red mud slurry is liquid-solid containing being 86g/L, and slurries main component is Na
2o
k108.51g/L, Al
2o
3113.75g/L, Na
2o
t129.67g/L.
Red-mud settlement and separation effect experimental is operating as: get red mud slurries that 200mL boils in the sedimentation pipe with a scale (φ 30 × 250mm) of 250mL, sedimentation pipe adds the flocculant solution of 0.1% of 50ppm embodiment product after being placed in the thermostatic glass water tank constant temperature 5min of 95 DEG C.The flocculant solution drawing certain volume with syringe is added in sedimentation pipe, lift up and down several times with self-control stainless steel mesh agitator, make flocculation agent blending dispersion even, press manual time-keeping simultaneously, the height that observed and recorded solid-liquid interface declines, surveys the turbidity of supernatant after sedimentation 30min.This experiment is with the settling velocity of the average settlement speed evaluation red mud in first 5 minutes of sedimentation, and supernatant layer height during sedimentation 5min and the ratio of settling time are front 5min average settlement speed.After sedimentation 30min, measure supernatant fluid turbidity with WGZ-3 type scattered light turbidimeter.
[table 1]
The flocculation agent of table 1 for preparing under differential responses pH condition, the relation of its hydroxamic acid, carboxyl-content and red-mud settlement and separation effect.
[table 2]
The flocculation agent of table 2 for preparing under differential responses temperature condition, the relation of its hydroxamic acid, carboxyl-content and red-mud settlement and separation effect.
[table 3]
The flocculation agent of table 3 for preparing under differential responses time conditions, the relation of its hydroxamic acid, carboxyl-content and red-mud settlement and separation effect.
As can be seen from table 1 table 3, relative contrast's example, the hydroxamic acid of the flocculation agent obtained by the present invention and the content of carboxyl all higher, settling velocity is faster, and effect of settling is better.
[table 4]
The flocculation agent prepared under the condition that table 4 is differential responses flow process, the relation of its hydroxamic acid, carboxyl-content and red-mud settlement and separation effect
As can be seen from Table 4, relative to the method being first hydrolyzed oxygen oximate again, the flocculation agent obtained by one pot process technique that hydroxamic acidization of the present invention and hydrolysis are carried out simultaneously, its Hydroxamic acid content, far above the former, is demonstrating better properties on the effect of settling of red mud.
Claims (7)
1. a preparation method for the flocculation agent of effective settlement separate high silicon high iron type Bayer process red mud, it is characterized in that, be dissolved in water polyacrylamide, obtains polyacrylamide solution; Under inert gas atmosphere, oxammonium hydrochloride is dissolved in NaOH solution, obtains hydroxylamine hydrochloride solution; Again by above-mentioned polyacrylamide solution and hydroxylamine hydrochloride solution mixing, reaction; In hydroxyamine groups in described oxammonium hydrochloride and polyacrylamide, the mol ratio of amide group is 1.2 ~ 1.5, and the pH in reaction process is 13 ~ 14, and temperature of reaction is 90 ~ 100 DEG C, and the reaction times is 24 ~ 48h; The limiting viscosity of polyacrylamide is 1200 ~ 1750mL/g.
2. method according to claim 1, is characterized in that, under inert gas atmosphere, oxammonium hydrochloride is dissolved in the NaOH solution of equimolar ratio.
3. method according to claim 1, is characterized in that, the matter average molecular weight of above-mentioned polyacrylamide is 2000 ~ 3,000 ten thousand.
4. method according to claim 1, is characterized in that, the pH in reaction process is by adding the sodium hydroxide solution adjustment that concentration is 20 ~ 40g/L.
5. method according to claim 1, is characterized in that, reacts while stirring in reaction process, and rotating speed during stirring is 45 ~ 60r/min.
6. method according to claim 1, is characterized in that, the rare gas element used is nitrogen.
7. the method according to any one of claim 1-5, it is characterized in that, after above-mentioned reaction completes, in reaction system, add dehydrated alcohol further, and close neutral to washings for several times with absolute ethanol washing, after 50 ~ 60 DEG C of drying 15 ~ 20h, obtain solid phase prod.
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| CN106583062A (en) * | 2017-01-09 | 2017-04-26 | 昆明理工大学 | Micro-fine particle tinstone selective flocculating agent and preparation method and application thereof |
| CN110950415B (en) * | 2019-11-29 | 2022-01-25 | 威海汉邦生物环保科技股份有限公司 | Biological polysaccharide-based heavy metal capture agent and preparation method thereof |
| CN111153423A (en) * | 2020-01-03 | 2020-05-15 | 江西理工大学 | Composite inhibitor containing PAH (polycyclic aromatic Hydroquinone) and preparation method and application thereof |
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