• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    The suspended solids content of Bayer process streams is reduced by contacting said stream with a polymer which contains hydroxamic acid groups.
    公开号:SU1687029A3
    申请号:SU884355165
    申请日:1988-02-10
    公开日:1991-10-23
    发明作者:С.Йен Вей；Пол Спицер Дональд
    申请人:Американ Цианамид Компани (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to the production of alumina by the Bayer method.
    The purpose of the invention is to increase the efficiency of the process.
    Obtaining polymer A.
    300 parts of a 20 wt.% - aqueous solution of a copolymer of acrylamide and acrylic acid (92/8) mol. M. 200,000 were mixed with 65.3 parts of hydroxylamine hydrochloride (65% excess based on copolymer amide groups), an equimolar amount (77.1 parts) of sodium acetate and water in an amount to bring the whole solution to 600 parts. The resulting solution was heated with stirring to 70-75 ° C for 5 hours. The infrared spectrum showed a conversion of 40% amide groups and hydroxamate groups.
    Obtaining polymer Century.
    100 parts of a 25% aqueous solution of homopolymer acrylamide, mol.m. 100,000 were mixed with 7.34 parts of hydroaxyl-min-hydrochloride (0.3 mol per 1 mole of amide), diluted to 80 parts, and 8.66 parts of sodium acetate, diluted to 70 parts. The pH was regulated and maintained at 6.5. The resulting solution was heated for 4 hours. A hydroxamated polyacrylamide was obtained.
    Example 1. Polymer B was added to a sump with a solution resulting from a Bayer plant for alumina production and mixed with stirring for 60 seconds. The solids were allowed to rest for 60 minutes to settle, while the solution was maintained at 95 ± 5 ° C. The sample was then removed from the upper part and tested by changing the absorbance at 900. The sample p / s was used to measure the time of the fig-trams) 0 ml through o and l of Whatman paper 54, the results are better. .eny in tabl, 1,
    A significant decrease in suspended solids is a result of the use of Polymer B, as can be seen from the reduced millimeters and increased filtration rates (Table 1),
    Example 2. Popmmer B was added with samples of the Bayer Grier 100 ° C clarifier solution in an amount of 0.020 g / l followed by the addition and without yoke of an industrial flocculant of red polyacrylate sludge. In both cases, fast flocculation and sedimentation of suspended solids were noted. particles. Measurement of suspended particles in the sludge showed that both samples contained about 5–10 ppm of suspended solids compared to 80–200 hr / million in a control sample using only the complete flocculus flocculant.
    Examples 3-7. Different doses of Polymaa A were injected into different samples of the product stream descending from a one-liter autoclave from an industrial r / inoeem production plant according to the Bayer process. Then, 3.1 liters of industry-produced 0.1% psc-heave were added - sodium liacrylate, the mixture was left at rest for 15 minutes to precipitate, part of the supernatant solution. The mixture was filtered with a millipore powder (0.45 µm) and the filtrate was analyzed for iron by atomic absorption spectroscopy. The results are shown in Table 2;
    As can be seen from tab. I, the use of half-A results in a significant decrease in the iron content of the sludge.
    Example B, A settler solution of an industrial installation according to the Bayer process was treated with industrial polycrylate as flocculant at a dosage equivalent to standard industry practice (control sample) or coated with polymer A and remained dormant for 15 days at 100 ° C. for 1. 2 and 4 hours. After sedimentation, 150 ml of sediment were carefully removed and mixed with 30 ml of alkaline solution, the HA was brought to a boil, the turbidity was cooled, and the turbidity was measured in a stream through the cell. It was found in her answer-lgvii with n: Muscle Calibration. The results Veda1 e table 3,
    As can be seen from Table 3, in all cases, polymer A is used to reduce the content of solids compared to standard flocculant,
    Examples 9-12. Polymer A i / Li B was added to the settler solution of an industrial plant for the production of alumina according to the Bayer process. In some cases, this addition was accompanied by agitation in the flocculant industrial plant in accordance with ACCEPTED practice. The treated solution was left alone to precipitate at 100 ° C for up to 3.5 hours. A portion of the resulting supernatant was then removed and its turbidity was measured {NTU - nephelometric turbidity unit). The results are shown in the table.
    The galvanometric measurement of suspended solids was carried out according to an industrial method on part of samples with very low turbidity values by adding 50 ml of an alkaline solution to 100 ml of solution, heating the resulting solution to a boil, filtering {0.5 µm), drying the resulting filter paper and residual, ashing dried material and weights. The results are shown in table.5.
    The examples show a decrease in turbidity compared with the use of industrial flocculant after an hour or more of the day.
    Examples 13-18. The settler solution from the other gummed installation according to the Beyers process was treated with polymer A and compared with the results achieved with a standard dosage of industrial floculant in the form of sodium polyacrylate. The reagents were mixed in a 50G ml sludge solution, the resulting solutions were precipitated at 100 ° C for 4 hours. Then, 100 ml sludge was collected, filtered and washed through a pre-weighed paper fiberglass hell, which was then dried and weighed to directly measure suspended particles. . The results are shown in table 6.
    It should be noted that the low amounts of half a mouth gel And 4 times the effect of lifeWith the normally used industrial floc nt,
    EXAMPLE 19-45. A series of suitable hydroxamated acrylamide polymers was prepared by adding sulfate-hydroxylamins to the polymer solution with the addition of choda. The pH was adjusted to b, C with 50% sodium hydroxide. Grinding is carried out at 0-75 ° C for 1-6 hours with the addition of 50% sulfuric acid if necessary to maintain a pH of 5 ± 0.5 to complete the reaction. Diluted (0.1 or 1.0%) aqueous solutions of the resulting hydroxamated polymers were then used to treat the settling solution (1 l each) from the industrial unit according to the Bayer process. Initial deposition rates were measured, after which the samples were maintained at 80 ° C for 60 minutes (deposition time). The final solids volume, turbidity and suspended solids content of the resulting sludge were then measured, the suspended solids were determined by filtering the top 250 ml through pre-weighed paper, followed by washing, drying and re-weighing. The results are shown in table.7.
    Examples 46-59. Additional precipitation tests were carried out similarly to Examples 19-45 using another settling solution (containing 10.5–23.9 g / l suspended solids) from a Bayer process plant using hydroxamated acrylamide polymer of different molecular weights. The precipitation time was limited to 30 minutes. Measurements of suspended solids were based on the ratio of the percent transmittance (transmission) at 910 nm relative to the number of suspended solids that was already installed in this industrial installation. The ratio was calibrated against only 94 mg / L (27% transmission), higher turbidity was determined by extrapolation. The results are shown in table.8.
    The achieved levels of suspended solids are low (5-10 mg / l), sedimentation rates are high (11.3 m / h).
    Examples 60-112. Using different polymers mentioned in the previous examples, precipitation tests were carried out with a sump solution (30-40 g suspended solids per liter) from an alumina production plant using a Bayer process using bauxite raw materials, which are known to give red mud with high surface area difficult to precipitate. The polymers were added to the settling solution in one cylinder of the cylinder, and the treated solutions were precipitated for 30 minutes at 90 ° C. The cylinders were mounted on slowly rotating (approximately 2 revolutions per minute) pillars to facilitate compaction. Samples of the precipitated solutions were taken from
    In the upper part, the turbidity was measured by the absorption method at 910 nm, which was converted into the amount (mg / l) of suspended solids using established industrial ratios. The results are given in table.9.
    Tests were also conducted in which the polymer was mixed with a settling solution and then the produced
    0 by industry, high molecular weight polyacrylate, The results are shown in Table 10.
    At relatively high doses of the polymer, good clearances were achieved, 1-2 mg of suspended solids per liter were observed (Table 9),
    As can be seen from Table 10, a number of combinations give very high deposition rates and much better clarity than
    0 using one industrial flocculant (examples 92 and 93 and examples 96, 101, 102 or 103).
    Examples 113-131. Additional polymers were prepared from aqueous solutions of polyacrylamide at the indicated ratios of NH20H (from hydroxylamine sulfate) to acrylamide. Enough NaOH was added for an initial pH of 6.0 and a final pH of 7.5-9.2. These polymers and different polymers from the preceding examples were tested on a sump solution in a Bayer unit, where the solution to be drained had a typical turbidity greater than NTU. Laboratory deposition tests with high power industrial polyacrylate with high molecular weight also showed high turbidity (217-232 NTU). Precipitation tests were carried out in one-liter cylinders when measuring the initial
    0, the deposition rate, then after 30 minutes at 80 ° C, part of the solution was removed from the upper layer, the turbidity was measured. The results are shown in table 11.
    Some of the treated solutions
    5 had a turbidity of 30 NTU or less, which is significantly better than in industrial practice (200 NTU or higher). Deposition rates are well above the required 5 ft / h and many more than 100 ft / h.
    0 Examples 132-134. The dosage of one of the reagents, following the procedure of examples 113-131, was reduced to 0.5 ppm (mg / l). Turbidity and precipitation rates are low. The results are given in Table 12.
    PRI me Era 135 and 136. Commercially available emulsion of polyacrylamide (mol.m. 15 million) reacted with equimolar equivalents of hydroxylamine (like hydroxylamine sulfate) and hydroxide.
    Catrick at 90 ° C for 20 hours. At the end of the reaction, the product was filled with a stable emulsion. Part of the product was diluted with water to concentrations of 0.1% (deige mineral gel). The settler solution was taken from a plant for the production of alumina according to the Bayer process, This solution contained 40 ± 4 mg of suspended matter:: respiratory particles n liter. In one-liter portions of this solution (gris 80 ± 5 ° С) different doses of the indicated 0.1% solution were injected. The start of the sedimentation rate was measured, then after 30 MfnH precipitation and a pen l nf.n 80 ° C a sample was taken from the upper g / o and the turbidity was measured. The results are shown in Table 13.
    Compared with the industrial Iraqi, this reagent gives improved clarity (transparency)
    EXAMPLE 137 and 100. The preparation was repeated with the exception that the initial emulsion was 70/30 copolymer of зcrylamide / acrylic / slots with moles of about 15 ppm, the amount of hydrosilamin used was exactly equivalent to the number of acrylics. The resulting product was tested with a solution of a Bayer sump, as in example pax 135 and 36. The results are presented in 18l 14
    Deposition rates and clarity were significantly better than in industrial practice.
    EXAMPLE 134-141. The proportion of 50.50 latex sogyulimomea phylamide / melakylaoylaga was obtained by reacting the monomers at 75 ° C, pH, 0 for 3 h with the aid of industrial surface-active substance and stabilizer used by ALI dispersion of methyl acrylate in a bottom arylamide solution. Both monomers were iggetally gradually, instead of with the oxidant, using a reducing system to the system. The obtained POTA is a gradual volumetric addition of a boiling (1BO ° C) solution of hydroxylamine sulfate and an EQUIE-Sodium amount of sodium hydroxide for 100 min. F I mol rs / droxylamine per 1 mol acrylate). A part of the obtained product was diluted with water to a concentration of 0.1% real pspimer. The settler pit (merged i autoclave autoclave with coarse calves removed / fj was removed from the alumina plant using the Bayer process). This solution contained 40 ± 4 g of suspended particles of palettes. Mixed o /) noliter portions of this solution (at 80 ± 5 ° C) administered different doses of the specified 0.1% solution. The initial-1 precipitation rate was measured.
    then the mixture was allowed to settle in an oven at 80 ° C for 30 minutes. At the end of this time, a sample was taken from the upper layer; turbidity was measured (this
    the sludge is a laboratories equivalent of the resulting sludge solution of an industrial plant). The results are presented in table 15.
    Although the deposition rates are rather unequal, the turbidity is much less than in the merged solution of an industrial installation.
    EXAMPLE 142-144. Prepared as in Examples 139-141, except for
    50:50 catalyst concentration was used for acrylamide / methyl acrylate latex in a ratio of 50:50. The resulting product was introduced into the settling solution in the Bayer process, as in Examples 135-141. The data are presented in Table 16.
    The deposition rates are acceptable, the turbidity is significantly less than in industrial practice (examples 139-141).
    Examples 145-147. Acrylic acid / methyl acrylate copolymer latex in a 75:25 ratio was formed gradually by adding a mixture of monomers and an oxidizing agent-1 z to a reducing catalytic system and water containing commercially available surfactants and stabilizers. The mixture was maintained at 75 ° C for 2 hours of reaction time. Then water solution
    hydroxylamine sulfate (1 mol hydroxylamine per 1 mol acryl eta) with an equivalent amount of NaOH was gradually introduced over 30 minutes into this latex at 100 ° C and the mixture was boiled for another 60
    min 0.1% aqueous solution is obtained from the mixture and tested for the deposition of solid particles and a solution of alumina Bayer, as in examples 139-141, the Results are presented in table 17.
    Examples 48-150. Preparations of Examples 145-147, Testing the deposition of solid particles in Bayer alumina solution, examples 139-141, were repeated. The results are presented in Table 18.
    Examples 151 and 152 (comparative).
    Preparations of Examples 145-H7 were repeated, except that the copolymer composition was 90:10 acrylic acid to methyl acrylate. The resulting copolymer mixture was a clear solution (not latex). The copolymer was reacted with hydroxylamine sulfate and NaOH (equivalent to the acrylate content) at 80 ° C for 1 hour. Testing for the deposition of solid particles in
    Bayer Alumina Solution. The results are presented in table 19.
    Poor results are caused by low methyl acrylate content and low conversion of this ester to hydroxamate. The polymer, as established (by NMR), contains undetectable hydroxamate (detection limit 1-2%). NMR also shows that the incorporation of methyl acrylate into the polymer was low.
    Examples 153 and 154. The preparations of Examples 145-147 were repeated, except that the resulting copolymer contained 50:50 acrylic acid / methyl acrylate. The copolymer product was a coarse dispersion of solid particles, which precipitated, if not mixed. Hydroxylamine sulfate and NaOH (equivalent to the acrylate content) were introduced into the dispersion and heated at 97 ° C for 1 hour to obtain a solution. The resulting polymer was tested against the deposition of solid particles in a solution of Bayer alumina, as before. The results are shown in Table 20.
    EXAMPLE 155 and 156. Acrylamide / methyl acrylate copolymer latex in a ratio of 25:75 was prepared and then reacted with hydroxylamine sulfate and NaOH, as in Examples 139-141. These reactions were followed by reaction with NaOH (3 hours at 95 ° C) to hydrolyze the unreacted ester. The final polymer was tested for the deposition of solid particles in a Bayer alumina solution. The results are shown in table.
    Example 157. A diluted (0.1%) polymer solution A. was added to a sample of a slurry slurry obtained from the last washing device of a washing line in a countercurrent solution undergoing decantation in a Bayer alumina plant in operation, and a rapid flocculation was noted. sedimentation of solid particles in suspension.
    Examples 158-161. The operations of Example 1 or 8 were repeated, except that different hydroxamated polymers replaced the polymers used for flocculation of solid particles from solutions. The results are shown in table 22.
    Mixtures of two or more hydroxamic acid containing polymers can be used together, combinations of hydroxamic acid containing polymers with other reagents can also be used together. Thus, with the proposed method, any polymer containing a group of water-soluble hydroxamic acid or salt can be used.
    The polymers can be illustrated by those that contain additional groups of the formula
    V
    -C-NH-OR
    where R is hydrogen or cation.
    These polymers are known in the art and may originate from polymers containing additional ester, amide, anhydride, nitrile, etc., as a result of reaction with hydroxylamine or its salt.
    5 Examples of polymers that can be hydroxy-modified for use in the process of the invention are polymers of acrylic, metatylic, crotonic and other acids,
    Polymers obtained as a result of the polymerization of methyl acrylate, ethyl acrylate, t-butyl acrylate, methyl methacrylate, ethyl methacrylate, cyclohexyl methacrylate, dimethylaminoethyl methacrylate, dimethyl 5 mino ethyl acrylate, methyl crotonate, and others, maleic anhydrides, polymethyl acrylate, dimethyl 5 mino ethyl acrylate, methyl acrotonate, and other, maleic anhydride polymers, dimethyl 5 mino ethyl acrylate, methyl crotonate, etc. are formed from acrylonitrile, etc., amide polymers such as
    Which are formed from acrylamide, metacrylamide, and the like. Hydroxylated polymers can be formed by reacting a mixture containing an additional reactive group in solution with
    5 hydroxylamine or its salt at a temperature in the range of 50-100 ° C for several hours. Approximately 1-90% of the possible additional reactive groups of the polymer may be substituted by hydroxyl groups.
    In addition to the reaction of hydroxylamine or its salt with a polymer solution, it was established that the polymer latex can react directly with hydroxyl 5 minutes or its salt. The latex may, for example, be a copolymer of acrylamide and methyl acrylate or a copolymer of acrylic acid and methyl acrylate. In these cases, hydrosylamine or its salt reacts
    0 primarily with ester groups to form hydroxamic acid groups.
    It was also found that inverse emulsions formed, for example, from liquid
    5 copolymers of polyacrylamide or acrylamide / acrylic acid, dispersed in oil, can be reacted directly with hydroxylamine or its salt to form very high molecular weight polymers containing
    hydroxamoic acid groups, which are all effective in the proposed method.
    The degree of hydroxamoarai, i.e. the concentration of the component in the above formula in polymers, mol and g (el in the range of 1-90 mol.%. (5-75, preferably 10-50 mol.%).
    The corresponding hydroxy amino salts include sulphates, sulphites, phosphates, perchlorates, hydrochlorides, acetates, propionates and goma-like, the pH of the solution is adjusted to 3-9, preferably above 6.0, by adding acid or base to the solution.
    Any water-soluble polymer can be used, which, after hydroxamination, functions in the direction of sedimentation of suspended solids. Thus, gmmopolymers, copolymers, gpolymers, and other specified monomers can be used. Corresponding comonomers, which by copolymerization can form, for example, up to 95% of the moles of the required polymers, can include acrypal acid, vinyl acetate, vinylpyrrolidone,, styrene, as well as other of pere-shc / one esters, amides and / or nitriles, etc., since such copolymers, terpolymers, etc. are water soluble after hydroxamination. My m of polymers 1x10 - 3x107.
    The polymers can be used by adding them, usually as a diluted water solution, to the product stream of digestible boxed raw material containing dissolved alumina and suspended solids dispersed in the solution, E, sufficient for precipitating suspended particles to obtain the best results. 0.1 mg hydroxautir & h of a polymer per liter of the product flow of the process (more godly (With mg mg hydrated polymer)) Mout and higher amounts are used, although aets point at which further quantities of HP gidroksametirovannogo polymer improves the separation rate, thus uneconomical isnepzovat excessively quantity.
    The method allows the cleaning efficiency to be achieved.
    Formula 1/1 of about (re e geni
    权利要求:
    Claims (15)
    [1]
    1, a method for separating suspended particles from Bayer process solutions by treating them with a water: TEOEIM polymer, characterized in that, in order to increase the effective process, the quality of the water-soluble polymer ISETHOL is a polymer containing hydroxamic acid groups or salts in the amount of 1-90 mol.% and having a molecular weight of 1 107.
    [2]
    2. A method according to claim 1, characterized in that derivatives of this polymer containing additional ester, amide, anhydride or nitrile groups are used as a water-soluble polymer containing hydroxamic acid groups or its salts.
    [3]
    3. A method according to claim 2, characterized in that a water-soluble polymer containing hydroxamic acid groups and its salts, as well as additional ester, amide, anhydride or nitrile groups, uses its derivative of the amide polymer.
    [4]
    4. A method according to claim 2, characterized in that a water-soluble polymer containing hydroxamic acid groups or ce salts, as well as additional ester groups (amide, anhydride, or nitrile, uses its derivative of acrylamide polymer.
    [5]
    5. A method according to claim 2, characterized in that the quality of a water-soluble polymer containing groups of hydroxamic acid and its salts, as well as additional groups of ester, amide, anhydride or nitrile, uses its derivative of the ester polymer,
    [6]
    6. A method according to claim 1, characterized in that the solution used for processing is a solution after settling the suspension in a sump.
    [7]
    7. Method according to claim 6, characterized in that after settling, the solution is fed to the treatment through the edge of the settler.
    [8]
    8. The method according to claim 1, wherein the process solution is a stream of leached pulp from the autoclave.
    [9]
    9. The method according to claim 2, wherein a water-soluble polymer containing hydroxamic acid groups or its salts, as well as additional ester, amide, anhydride, or nitrile groups, uses derivatives of polymer a, phi-meta or meta-acylate.
    [10]
    10. The process according to claim 1, wherein the water-soluble polymer is used in the form of an emulsion,
    [11]
    11. A method according to claim 1, characterized in that a polymer containing hydroxamic acid groups or its salt E is used as the water-soluble half polymer, E is 5-75 mol%.
    [12]
    12. The process according to claim 1, wherein a water-soluble polymer is a polymer containing hydroxamic acid groups or its salt in an amount of 10-50 mol%.
    [13]
    13. The method according to claim 1, characterized in that the water-soluble polymer is used together with an anionic flocculant.
    [14]
    14. A method according to claim 13, characterized in that a salt of a polyacrylate polymer is used as an anionic flocculant.
    [15]
    15. Method according to claim 13, characterized in that a copolymer of an acrylate salt with acrylamide is used as an anionic flocculant.
    Table 1
     An industrial flocculant was also added 2 minutes after polymer A or B.
    table 2
    Table 3
    Table 4
    polymer
    Dosage,
    ppm
    A B A
    20 20 40
    The molar percentage of the hydroxplexic acid groups, the numbers in the slots and the general public, use the acids, the rest is nzr special transcription of the acid).
    11 I (. Mln is approximately equal to tO g / t lunnMomix tverp 0 pgtnts. Tg sting POBG p s rastnost rastela early standard train osdmi.
    Table 5
    Table 6
    T a b l and c a -7
    Reagent
    Mol.m.
    NH OH-AM, mol.
    46100K
    47200K
    48200K

    420K 420K 600K 600K
    600K 800K
    200K 1.5
    200K 2.0
    420K 1.0
    1.5 2.0 1.0 1.5
    2.0 1.0
    800K 1.5 800K 2.0
    defined P
    23
    40. 4.5
    not . defined .-
    Not defined
    Plus the equivalent of sodium acetate.
     /
    89,100
    66
    73
    88
    43.68 62.76 94
    100 150
    76 81
    3.6 60
    Undetermined / 35 ..- 1. -
    3.7 6.4 Not
    definition „-
    Not defined
    44 48 No
    defined and
    Not defined
    4.3 8.0 Not
    defined and
    4.3 7.6 Not
    defined
    Not defined
    100
    6.7 5.9
    26.22 3.8 27.11 4.3 5
    Not defined Not defined Not defined
    -
    8 th go with
    63
    71
    54
    00
    Preparation, as in Example 54, except that the reaction was carried out entirely with pI 3-4.
    Prepared as in Example 53, with the exception that the reaction was carried out completely at pH 3-4,
    1687029
    20 T a b i c a 9
    Table 10
    Example
    Polymer content, mg / l
    Sump work
    installations
    135
    136
    Minimum requirement
    C, polymer lambing, mg / l
    2
     Minimum requirement
    Table 12
    Table 13
    Table 14
    Table 15
    Table 16
    Note. AM - acrylamide, DMAEM - dimethylaminoethylacrylate.
    MMA - Methyl Methacrylate, MA - Maleic Anhydride, PAN - Polyethylaminate - Motor Mold Qttiun
    lҐiivir i mv i plgpo I ai | jri / ici I, rna / ti rinwDwtri
    acrylonitrile, MVE - methyl vinyl ether.
    Table 18
    Table 19
    Table 20
    Table 21
    Table 22
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    引用文献:
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    申请号 | 申请日 | 专利标题
    US07/013,491|US4767540A|1987-02-11|1987-02-11|Polymers containing hydroxamic acid groups for reduction of suspended solids in bayer process streams|
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