CN104668102A - Obverse flotation collecting agent for low temperature-resistant collophanite and preparation method thereof - Google Patents
Obverse flotation collecting agent for low temperature-resistant collophanite and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an obverse flotation collecting agent for low temperature-resistant collophanite and a preparation method thereof. The preparation method comprises the following technological steps of using plant oil residue acidified oil fatty acid as a raw material, utilizing a urea inclusion fractionating method to remove the saturated fatty acid with high melting point and low solubility, and preparing liquid acid with iodine value range of 140-165I2/100g, low melting point and high solubility and without saturated fatty acid; adding NaOH (sodium hydroxide) into the liquid acid to saponify, and then adding an additive, so as to obtain the obverse flotation collecting agent for the low temperature-resistant collophanite. The obverse flotation collecting agent for the low temperature-resistant collophanite has the characteristics that the chemical property is stable, the low temperature-resistant property is good, the solution and dispersing properties in water are good, the usage amount is less, the collecting property is strong, the selectivity is good, and the like; the grade of the concentrate can be effectively improved at the lower flotation temperature, and the content of impurities of the concentrate product can be reduced.
Description
Technical field
The present invention relates to a kind of collophane direct flotation collecting agent, particularly relate to a kind of method preparing the low temperature resistant direct flotation collecting agent of collophane not containing high-melting-point saturated fatty acid.
Background technology
In phosphate rock floating, external conventional collecting agent is tall oil, oleic acid and saponified, and China's major part is all use sodium soap.Aliphatic acid majority as flotation collector comes from natural plant grease, but the aliphatic acid of different vegetable fat composition has larger difference because of the difference of kind.Therefore the fatty acid collecting agent used in phosphate rock floating process is also because of difference of originating, and its aliphatic acid composition has larger difference.Through experimental studies have found that different aliphatic acid sorts larger difference for phosphorus ore.Aliphatic acid can be divided into saturated fatty acid and unrighted acid with its saturation degree, wherein saturated fatty acid through the saturated fatty acid sodium of saponification gained dissolve in water and dispersiveness poor, and unrighted acid sodium has relatively high solubility and dispersiveness in water.In collophane direct flotation, fatty acid collecting agent and collophane are had an effect by chemisorbed, require that collecting agent used has good solubility and dispersiveness in water.The character of saturated fatty acid dissolubility and bad dispersibility in water, makes usually mixed type fatty-acid collector used have poor solubility and dispersiveness, and when slurry temperature is lower, the performance of this phenomenon is more obvious.Therefore, when northern area water temperature is lower than 15 DEG C in the winter time, ore pulp needs ability flotation of heating, and even some ore dressing plant ore pulp is heated throughout the year, and flotation energy consumption is large.
Summary of the invention
The object of the invention is for prior art defect, provide a kind of raw material sources extensively, stable in properties, collecting power and selective good, the collophane low temperature resistant direct flotation collecting agent preparation method of slurry temperature wide accommodation.
The present invention's low temperature resistant collophane direct flotation collecting agent and preparation method thereof concrete technology step is: (1) urea clathrate divides carries aliphatic acid: joined by appropriate urea in a certain amount of 95% ethanol, add hot reflux, after urea all dissolves, add a certain amount of vegetable oil residue acidification oil aliphatic acid by a certain percentage, stir, water-bath refluxes after 30 min ~ 60min, cool to room temperature, then under different temperatures, in Water Tank with Temp.-controlled, a period of time is preserved in water-bath, explosive decompression suction filtration after taking out, appropriate petroleum ether extraction is added in filtrate, get oil reservoir, rotary evaporation removing benzinum obtains the liquid acid not containing saturated acid,
(2) interpolation of the saponification of saturated fatty acid liquid acid and auxiliary agent is not contained: in this liquid acid, add a certain amount of water and caustic soda, carry out saponification 60 min ~ 90min in 100 DEG C ~ 110 DEG C.Add again after saponification terminates and account for the auxiliary agent that liquid acid weighs 3% ~ 15% and namely obtain low temperature resistant collophane direct flotation collecting agent.
In described step (1), the acid number of vegetable oil residue acidification oil hydrolyzed fat acid is 170mgKOH/g ~ 195mgKOH/g, and iodine number is 105gI
2/ 100g ~ 130gI
2/ 100g.
Described step (1) urea divides in the process of carrying, and each material proportion is urea (g): aliphatic acid (g): 95% ethanol (mL)=(0.8 ~ 2): 1:(2 ~ 5), inclusion temperature-10 DEG C ~ 15 DEG C, inclusion time 3h ~ 12h.
Described step (1) urea clathrate gained liquid acid iodine number scope is 140gI
2/ 100g ~ 165gI
2/ 100g, wherein saturated fatty acid content is not for detect, and oleic acid content is 10% ~ 30%, and linoleic acid content is 45% ~ 70%, and linolenic acid content is 3% ~ 15%.
During described step (2) liquid acid saponification add NaOH amount be 14% ~ 18% of base stock weight.
The addition of described step (2) auxiliary agent be raw material liq acid heavy 3% ~ 15%.
Described step (2) auxiliary agent is the mixture of 8 carbon straight chain alcohols and branched-chain alcoho and ester class.
The present invention adopts urea adduct method to divide and carries aliphatic acid, can remove the saturated fatty acid in vegetable oil residue acidification oil aliphatic acid completely, to improve the dissolution in low temperature performance and dispersiveness that remove gained sodium soap after saturated acid, improves the flotation at low temperature adaptability of collecting agent.And common point of extracting method is carried as dry fractionation, solvent divide, emulsification divides and carries, and point extracting method such as distilation all can not remove the saturated fatty acid in common fats acid completely.
Compared with existing fatty acid collecting agent of the same type, the present invention has the following advantages:
1. the urea that urea clathrate is used, 95% ethanol and benzinum all can be recycled, and the solid acid part produced also can use as mineral collector, does not have waste liquid to discharge in medicament preparation process.
2. can, according to the change of ore properties and process conditions, regulate urea saturation conditions to obtain the collecting agent of applicable aliphatic acid composition.
3. the direct flotation collecting agent prepared by has good low temperature adaptability, 5 DEG C time, still have good sorting adaptability.Solve the problem of common fats acid collector low temperature separation performance difference, thus flotation can be carried out at low temperatures, for phosphorus ore continuous production of not heating the whole year provides guarantee.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, but be not limited to embodiment.
Low temperature resistant collecting agent of collophane direct flotation of the present invention and preparation method thereof adopts following technology and step to carry out: urea clathrate divides carries aliphatic acid: joined by appropriate urea in a certain amount of 95% ethanol, add hot reflux, after urea all dissolves, add the acid of a certain amount of vegetable oil residue acidification oil hydrolyzed fat by a certain percentage, stir, water-bath refluxes after 30 min ~ 60min, cool to room temperature, then under different temperatures in Water Tank with Temp.-controlled water-bath inclusion a period of time, explosive decompression suction filtration after taking out, appropriate petroleum ether extraction is added in filtrate, get oil reservoir, rotary evaporation removing benzinum obtains the liquid acid not containing saturated acid.
Do not contain the interpolation of the acid saponification of inclusion fatty acid liquid and auxiliary agent: in this liquid acid, add a certain amount of water and caustic soda, carry out saponification 60 min ~ 90min in 100 DEG C ~ 110 DEG C.Add again after saponification terminates and account for the auxiliary agent that liquid acid weighs 3% ~ 15% and namely obtain low temperature resistant collophane direct flotation collecting agent.
Parameter involved by above-mentioned technology and step and raw material and product property as follows:
The acid number of material plant oil foot acidification oil hydrolyzed fat acid is 170mgKOH/g ~ 195mgKOH/g, and iodine number is 105gI
2/ 100g ~ 130gI
2/ 100g.
Described urea divides each material proportion in the process of carrying to be urea: aliphatic acid: 95% ethanol (g/g/mL)=(0.8 ~ 2): 1:(2 ~ 5), inclusion temperature-10 DEG C ~ 15 DEG C, inclusion time 3h ~ 12h.Urea clathrate gained liquid acid iodine number scope is 140gI
2/ 100g ~ 165gI
2/ 100g, wherein saturated fatty acid content is not for detect, and oleic acid content is 10% ~ 30%, and linoleic acid content is 45% ~ 70%, and linolenic acid content is 3% ~ 15%.
During described liquid acid saponification add NaOH amount be 14% ~ 18% of base stock weight, amount of water is 3 times of aliphatic acid and NaOH weight sum.
The addition of described auxiliary agent be raw material liq acid heavy 3% ~ 15%.The classification of auxiliary agent is the mixture of 8 carbon straight chain alcohols and branched-chain alcoho and ester class.
Embodiment 1-4 sees the following form 1.
Table 1 low temperature resistant collophane direct flotation collecting agent preparation condition and pulp furnish
In table 1: the acid of A-vegetable oil residue acidification oil hydrolyzed fat; B-urea; C-95% ethanol.The iodine number of vegetable oil residue acidification oil hydrolyzed fat acid is: 123gI
2/ 100g, acid number is 190mgKOH/g.Stable in properties, collecting ability and selective good collophane direct flotation collecting agent under cryogenic conditions all can be obtained by upper table embodiment.
Collophane collecting agent flotation example of the present invention illustrates:
1, the siliceous collophane in Yunnan, P
2o
5content is 21.08%, SiO
2content is 34.80%, and when water temperature is 15 DEG C, the application embodiment of the present invention 3 medicament is direct flotation collecting agent, and adopt a thick smart open circuit flows flow process, collector dosage is 2.0Kg/t raw ore, and floatation indicators is concentrate P
2o
5grade 26.18%, SiO
2content is 22.02%, mine tailing P
2o
5grade 13.08%, P
2o
5the rate of recovery is 72%, and desiliconization rate 42.58%, effectively improves P
2o
5grade, reaches and falls the object that silicon carries phosphorus.
2, use oleic acid and Collectors for Phosphorous Ore of the present invention to certain siliceous collophane (P of flotation example 1
2o
5content is 21.08%, SiO
2content is 34.80%) carry out under identical experiment condition direct flotation roughly select temperature comparisons test, comparing result is in table 2, and the medicament of employing is embodiment 3.
Table 2 oleic acid and collophane collecting agent flotation temperature comparing result of the present invention
Shown from collecting agent flotation temperature comparing result of the present invention by table 2 oleic acid: under different slurry temperatures, collecting agent of the present invention is compared with enuatrol, and under identical regime of agent, when temperature is higher, collecting agent collecting ability of the present invention is strong, concentrate grade comparatively oleic acid is low, but rate of recovery ratio oleic acid is high.Along with temperature declines, the advantage of collecting agent of the present invention just displays, and when temperature is down to 5 DEG C, collecting agent concentrate grade of the present invention is higher than oleic acid, and the concentrate rate of recovery is 76.27%, and the oleic acid concentrate rate of recovery drops to 48.84%.Visible, collecting agent of the present invention is to the strong adaptability of temperature, and when flotation at low temperature collophane, adaptability is better.
Claims (7)
1. low temperature resistant collophane direct flotation collecting agent and preparation method thereof, is characterized in that concrete technology step is:
(1) urea clathrate divides and carries aliphatic acid: joined by appropriate urea in a certain amount of 95% ethanol, add hot reflux, after urea all dissolves, add a certain amount of vegetable oil residue acidification oil aliphatic acid by a certain percentage, stir, water-bath refluxes after 30 min ~ 60min, cool to room temperature, then under different temperatures, in Water Tank with Temp.-controlled, a period of time is preserved in water-bath, explosive decompression suction filtration after taking out, in filtrate, add appropriate petroleum ether extraction, get oil reservoir, rotary evaporation removing benzinum obtains the liquid acid not containing saturated acid;
(2) interpolation of the saponification of saturated fatty acid liquid acid and auxiliary agent is not contained: in this liquid acid, add a certain amount of water and caustic soda, carry out saponification 60 min ~ 90min in 100 DEG C ~ 110 DEG C, add again after saponification terminates and account for the auxiliary agent that liquid acid weighs 3% ~ 15% and namely obtain low temperature resistant collophane direct flotation collecting agent.
2. a kind of low temperature resistant collophane direct flotation collecting agent as claimed in claim 1 and preparation method thereof, it is characterized in that the acid number of vegetable oil residue acidification oil hydrolyzed fat acid in described step (1) is 170mgKOH/g ~ 195mgKOH/g, iodine number is 105gI
2/ 100g ~ 130gI
2/ 100g.
3. one according to claim 1 low temperature resistant collophane direct flotation collecting agent and preparation method thereof, it is characterized in that described step (1) urea divides in the process of carrying, each material proportion is urea (g): aliphatic acid (g): 95% ethanol (mL)=(0.8 ~ 2): 1:(2 ~ 5), inclusion temperature-10 DEG C ~ 15 DEG C, inclusion time 3h ~ 12h.
4. one according to claim 1 low temperature resistant collophane direct flotation collecting agent and preparation method thereof, is characterized in that described step (1) urea clathrate gained liquid acid iodine number scope is 140gI
2/ 100g ~ 165gI
2/ 100g, wherein saturated fatty acid content is not for detect, and oleic acid content is 10% ~ 30%, and linoleic acid content is 45% ~ 70%, and linolenic acid content is 3% ~ 15%.
5. one according to claim 1 low temperature resistant collophane direct flotation collecting agent and preparation method thereof, when it is characterized in that described step (2) liquid acid saponification add NaOH amount be 14% ~ 18% of base stock weight.
6. one according to claim 1 low temperature resistant collophane direct flotation collecting agent and preparation method thereof, is characterized in that the addition of described step (2) auxiliary agent is that raw material liq acid is heavy by 3% ~ 15%.
7. one according to claim 6 low temperature resistant collophane direct flotation collecting agent and preparation method thereof, is characterized in that described step (2) auxiliary agent is the mixture of 8 carbon straight chain alcohols and branched-chain alcoho and ester class.
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| CN201510103099.2A CN104668102B (en) | 2015-03-10 | 2015-03-10 | A kind of low temperature resistant Cellophane direct flotation collecting agent and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107309095A (en) * | 2017-06-05 | 2017-11-03 | 武汉工程大学 | A kind of collophane low temperature direct flotation Compositional type collecting agent and preparation method thereof |
| CN108722676A (en) * | 2018-05-31 | 2018-11-02 | 广东省资源综合利用研究所 | A kind of collecting agent and its preparation method and application |
| CN109482354A (en) * | 2018-11-16 | 2019-03-19 | 西北矿冶研究院 | Novel combined collecting and foaming agent for sorting copper ores in alpine regions and application thereof |
| CN111001496A (en) * | 2019-12-31 | 2020-04-14 | 云南磷化集团有限公司 | Collophanite flotation collector prepared from vegetable oil fatty acid |
| CN115739401A (en) * | 2022-11-07 | 2023-03-07 | 盐亭优锂新材料科技有限公司 | Treatment method for improving storage time and collecting effect of collecting agent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107309095A (en) * | 2017-06-05 | 2017-11-03 | 武汉工程大学 | A kind of collophane low temperature direct flotation Compositional type collecting agent and preparation method thereof |
| CN108722676A (en) * | 2018-05-31 | 2018-11-02 | 广东省资源综合利用研究所 | A kind of collecting agent and its preparation method and application |
| CN109482354A (en) * | 2018-11-16 | 2019-03-19 | 西北矿冶研究院 | Novel combined collecting and foaming agent for sorting copper ores in alpine regions and application thereof |
| CN111001496A (en) * | 2019-12-31 | 2020-04-14 | 云南磷化集团有限公司 | Collophanite flotation collector prepared from vegetable oil fatty acid |
| CN111001496B (en) * | 2019-12-31 | 2022-04-12 | 云南磷化集团有限公司 | Collophanite flotation collector prepared from vegetable oil fatty acid |
| CN115739401A (en) * | 2022-11-07 | 2023-03-07 | 盐亭优锂新材料科技有限公司 | Treatment method for improving storage time and collecting effect of collecting agent |
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