CN108144752A - A kind of rare earth catching agent formula and preparation method thereof - Google Patents
A kind of rare earth catching agent formula and preparation method thereof Download PDFInfo
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- CN108144752A CN108144752A CN201711388436.2A CN201711388436A CN108144752A CN 108144752 A CN108144752 A CN 108144752A CN 201711388436 A CN201711388436 A CN 201711388436A CN 108144752 A CN108144752 A CN 108144752A
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- rare earth
- furfural
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
Abstract
The invention discloses a kind of rare earth catching agent formula and preparation method thereof, the group ingredient including following weight percent：Hydroxyl 40%~70%, naphthoic acid 10%~20%, formaldehyde 5%~10%, furfural 10%~20%, beauteously sub- orchid 2%~10%, alkane kerosene 5%~10%, the concentrated sulfuric acid 5%~10%, sodium hydroxide 2%~10%, hydroxylamine hydrochloride 5%~15%.Furfural is set, it is active by the chemical property of furfural, numerous derivatives can be produced by the reactions such as aoxidizing, being condensed, and furfural is a kind of benefit of good extractant simultaneously, advantageously allows the effect of rare earth catching agent interior molecules are enlivened, improve rare earth catching agent；Hydroxyl is one of most common functional group in organic chemistry simultaneously, and either alcoholic extract hydroxyl group or phenolic hydroxyl group is easily aoxidized by a variety of oxidants, improves the rate of recovery of rare earth catching agent.
Description
Technical field
The present invention relates to a kind of rare earth catching agents, and in particular to a kind of rare earth catching agent formula and preparation method thereof.
Background technology
Rare earth has the laudatory title of " industrial vitamin ".Nowadays extremely important strategic resource has been become.Rare earth element aoxidizes
Object refer to period of element atom ordinal number be 57 to 71 15 kinds of lanthanide oxides and with lanthanide series chemical property
The oxide of similar scandium and yttrium totally 17 kinds of elements.Rare earth element is in oil, chemical industry, metallurgy, weaving, ceramics, glass, permanent magnetism material
The fields such as material are obtained for and are widely applied, with advances in technology with the continuous breakthrough of application technology, the valency of rare earth oxide
Value will be increasing.Rare earth leading enterprise, northern rare earth are issued《The bulletin supported value about limited production》.Bulletin display, in view of working as
The continued downturn of preceding rare earth market, the situation of the long-term low level of product price for China's Rare-earth Industry is promoted to develop in a healthy way, are effectively alleviated
The rare earth demand and supply contraction, northern rare earth determine that implementing limited production supports value, and whole year smelts separation amount of product throughput and assigned compared with Ministry of Industry and Information
10% or so is reduced to total amount of rare earth control plan index amounts in 2015 of company.According to rare earth atoms electron structure and
Physicochemical properties and their symbiosis situation and different ionic radius in mineral can generate feature of different nature, and ten
Seven kinds of rare earth elements are generally divided into two groups：Light rare earth includes：Lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium.Heavy rare earth includes：Gadolinium, terbium, dysprosium,
Holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium.But existing rare earth catching agent structure is more single, relatively low to rougher concentration grade rank, simultaneously
It is relatively low to the rate of recovery of rare earth, cause using trouble, the problem of material wastes.
Invention content
The technical problem to be solved by the present invention is to overcome existing rare earth catching agent structure it is more single, to rougher concentration
The problem of grade rank is relatively low, while relatively low to the rate of recovery of rare earth, causes using trouble, and material wastes, provides a kind of rare earth
Collecting agent prescription.
In order to solve the above technical problem, the present invention provides following technical solutions：
The present invention provides a kind of rare earth catching agent formula, the group ingredient including following weight percent：Hydroxyl 40%~
70%, naphthoic acid 10%~20%, formaldehyde 5%~10%, furfural 10%~20%, beauteously sub- orchid 2%~10%, alkane kerosene
5%~10%, the concentrated sulfuric acid 5%~10%, sodium hydroxide 2%~10%, hydroxylamine hydrochloride 5%~15%.
As a preferred technical solution of the present invention, the preparation method is as follows：
Step 1：Hydroxyl, naphthoic acid and the concentrated sulfuric acid are added in three-necked flask by a certain percentage, are sufficiently stirred 5~10 points
Clock forms it into yellow solution；
Step 2：By the concentrated sulfuric acid by the solution described in a small amount of addition step 1 of dropping funel, standing 3~5 minutes；
Step 3：Solution described in step 2 is heated to reflux 24~48 hours, solution is made to react completely；
Step 4：Solution described in step 3 is poured into beaker, is placed 8~12 hours, solution crystallization is complete；
Step 5：Crystallization described in step 4 is filtered off into mother liquor, water washing is added to dry in the air at a temperature of 22 °~26 ° into neutrality
It is dry；
Step 6：It will beauteously Ya Lan and alkane kerosene be put into agitator, be stirred 10~15 minutes, after stirring evenly
Pour into flask；
Step 7：Crystallization described in step 5 is put into reaction kettle, pure water is added in and is stirred 5~10 minutes；
Step 8：Flask contents described in step 6 are poured into the reaction kettle described in step 7, are stirred 5~10
Minute；
Step 9：Furfural and hydroxylamine hydrochloride are added in the reaction kettle described in step 8,40 °~60 ° of heating and react 3~
6 hours, it is cooled to 8 °~30 ° after reaction, is diluted with water.
As a preferred technical solution of the present invention, the reaction kettle is enamel reaction still.
As a preferred technical solution of the present invention, the naphthoic acid, the formaldehyde, the sodium hydroxide and the salt
Sour azanol is industrial rank.
As a preferred technical solution of the present invention, the furfural extracting method：Using bagasse as raw material, using dilute sulphur
Acid catalyst in hydrolytic process, will hydrolyze the furfural generated with high-pressure steam and other by-product volatile materials bands is discharged
Pot is solved, forms aldehyde gas.Generally 4-6% containing furfural in aldehyde gas, acetic acid 1_2%, also a small amount of low-boiling-point substance.Enter after aldehyde gas is condensed
First gold-plating tower obtains furfural azeotrope with water object in tower top, and first gold-plating bottom of towe discharges furfural.
As a preferred technical solution of the present invention, the hydroxyl extracting method：Carboxyl compound plant is added into water
It crushes, destroys plant cell wall, beta-glucosidase degradation desugar, hot alkaline water dissolving adds cationic surfactant chemical combination
Reaction stirring, cooling, hydrochloric acid reaction reduction, freeze-drying.
As a preferred technical solution of the present invention, the hydroxylamine hydrochloride nitrous acid preparation method is as follows：Sodium synthetic method
Reaction kettle is added water to, sodium nitrite is added with stirring, adds in sodium pyrosulfite by several times, be then acidified with sulfuric acid.After being acidified
Material be sent into hydrolysis kettle, add in acetone, then neutralized with liquid caustic soda, neutralizer is distilled, obtains acetoxime.Acetoxime and hydrochloric acid are added
Enter into salt oven and react, generate hydroxylamine hydrochloride and acetone.Acetone recycling uses；Hydroxylamine hydrochloride is concentrated, crystallisation by cooling, centrifuges and divides
From, it is dry to get finished product
In technical scheme of the present invention, the chemical property of furfural is active, can by aoxidize, be condensed etc. reactions produce it is numerous
Derivative；Furfural is a kind of good extractant, since the ether of the carbon-based of furfural, double bond and furan nucleus constructs, makes furfural anti-
It should be very capable.Pure furfural boils in 1 bar of atmospheric pressure and 161.7 DEG C, is colourless oily liquids, is there is situation existing for acid
Lower esterification, it is easily utilized without poison；Furfural is fabulous organic solvent simultaneously, can accelerate the reaction of solvent.Hydroxyl
With good reproducibility, aldehydes or ketones or carboxylic acid can be oxidized to；There is faintly acid simultaneously, phenolic hydroxyl group reacts life with sodium hydroxide
Into phenol sodium.Although in slant acidity, the aqueous solution acidity of many hydroxyl organic matters is weaker than water.Hydroxyl be in organic chemistry most
One of common functional group, either alcoholic extract hydroxyl group or phenolic hydroxyl group are easily aoxidized by a variety of oxidants.Therefore multifunctional
In the building-up process of group's compound, hydroxyl or part of hydroxyl need first to be protected, it are prevented to participate in reaction, in proper step
In be converted again.In inorganic matter, it is oxyacid or its acid salt to usually contain hydroxyl.The substance of hydroxyl is dissolved in water
Hydrogen ion can be ionized out, therefore the substance aqueous solution of hydroxyl is mostly into slant acidity.In the systematic naming method of organic chemistry in organic matter
In, it is referred to as alcohol in simple alkyl followed by hydroxyl, and carbohydrate is mostly polyhydroxy aldehydes or ketones.
The advantageous effect that is reached of the present invention is：The device is a kind of rare earth catching agent formula, sets furfural, passes through furfural
Chemical property it is active, can producing numerous derivatives by the reactions such as aoxidizing, being condensed, furfural is a kind of extraction well simultaneously
The benefit of agent is taken, advantageously allows the effect of rare earth catching agent interior molecules are enlivened, improve rare earth catching agent；Hydroxyl is simultaneously
One of most common functional group in organic chemistry, either alcoholic extract hydroxyl group or phenolic hydroxyl group are easily aoxidized by a variety of oxidants.
Therefore in the building-up process of polyfunctional compound, hydroxyl or part of hydroxyl need first to be protected, it is prevented to participate in reaction,
Be conducive to improve the rate of recovery of rare earth catching agent, provide a kind of rare earth catching agent formula.Reasonable design of the present invention, structure letter
It is single, safe and reliable, easy to use, easy to maintain, it has good value for applications.
Specific embodiment
It is illustrated below in conjunction with to the preferred embodiment of the present invention, it should be understood that preferred embodiment described herein
It is merely to illustrate and explain the present invention, is not intended to limit the present invention.
Embodiment 1
The present invention provides a kind of rare earth catching agent formula, the group ingredient including following weight percent：Hydroxyl 40%, naphthalene first
Acid 10%, formaldehyde 5%, furfural 10%, beauteously sub- orchid 2%, alkane kerosene 5%, the concentrated sulfuric acid 5%, sodium hydroxide 2%, hydrochloric acid hydroxyl
Amine 5%.
As a preferred technical solution of the present invention, preparation method is as follows：
Step 1：Hydroxyl, naphthoic acid and the concentrated sulfuric acid are pressed 3:2:1 ratio is added in three-necked flask, is sufficiently stirred 5 minutes,
Form it into yellow solution；
Step 2：By in solution of the concentrated sulfuric acid by a small amount of addition step 1 of dropping funel, 3 minutes are stood；
Step 3：The solution of step 2 is heated to reflux 24 hours, solution is made to react completely；
Step 4：The solution of step 3 is poured into beaker, is placed 8 hours, solution crystallization is complete；
Step 5：The crystallization of step 4 is filtered off into mother liquor, water washing is added to be dried at a temperature of 22 ° into neutrality；
Step 6：It will beauteously Ya Lan and alkane kerosene be put into agitator, and be stirred 10 minutes, poured into after stirring evenly
Flask；
Step 7：The crystallization of step 5 is put into reaction kettle, pure water is added in and is stirred 5 minutes；
Step 8：The flask contents of step 6 are poured into the reaction kettle of step 7, be stirred 5 minutes；
Step 9：Furfural and hydroxylamine hydrochloride are added in the reaction kettle of step 8,40 ° of heating is simultaneously reacted 5 hours, reaction knot
Beam postcooling is diluted with water to 24 °.
Furfural extracting method：Using bagasse as raw material, using dilute sulfuric acid catalyst, in hydrolytic process, steamed with high pressure water
Gas will hydrolyze the furfural generated and other by-product volatile materials take hydrolyzer out of, form aldehyde gas.Generally 4- containing furfural in aldehyde gas
6%, acetic acid 1_2%, also a small amount of low-boiling-point substance.Enter first gold-plating tower after aldehyde gas is condensed, furfural azeotrope with water object obtained in tower top,
First gold-plating bottom of towe discharge furfural.
Hydroxyl extracting method：Add pigment broken carboxyl compound plant, destroy plant cell wall, beta-glucosidase drop
Desugar is solved, hot alkaline water dissolving adds cationic surfactant combination reaction to stir, cooling, hydrochloric acid reaction reduction, freeze-drying
.
Embodiment 2
The present invention provides a kind of rare earth catching agent formula, the group ingredient including following weight percent：Hydroxyl 50%, naphthalene first
Acid 8%, formaldehyde 6%, furfural 15%, beauteously sub- orchid 2%, alkane kerosene 5%, the concentrated sulfuric acid 5%, sodium hydroxide 2%, hydroxylamine hydrochloride
5%.
As a preferred technical solution of the present invention, preparation method is as follows：
Step 1：Hydroxyl, naphthoic acid and the concentrated sulfuric acid are pressed 3:1:1 ratio is added in three-necked flask, is sufficiently stirred 5 minutes,
Form it into yellow solution；
Step 2：By in solution of the concentrated sulfuric acid by a small amount of addition step 1 of dropping funel, 3 minutes are stood；
Step 3：The solution of step 2 is heated to reflux 24 hours, solution is made to react completely；
Step 4：The solution of step 3 is poured into beaker, is placed 8 hours, solution crystallization is complete；
Step 5：The crystallization of step 4 is filtered off into mother liquor, water washing is added to be dried at a temperature of 22 ° into neutrality；
Step 6：It will beauteously Ya Lan and alkane kerosene be put into agitator, and be stirred 10 minutes, poured into after stirring evenly
Flask；
Step 7：The crystallization of step 5 is put into reaction kettle, pure water is added in and is stirred 5 minutes；
Step 8：The flask contents of step 6 are poured into the reaction kettle of step 7, be stirred 5 minutes；
Step 9：Furfural and hydroxylamine hydrochloride are added in the reaction kettle of step 8,40 ° of heating is simultaneously reacted 5 hours, reaction knot
Beam postcooling is diluted with water to 24 °.
Furfural extracting method：Using bagasse as raw material, using dilute sulfuric acid catalyst, in hydrolytic process, steamed with high pressure water
Gas will hydrolyze the furfural generated and other by-product volatile materials take hydrolyzer out of, form aldehyde gas.Generally 4- containing furfural in aldehyde gas
6%, acetic acid 1_2%, also a small amount of low-boiling-point substance.Enter first gold-plating tower after aldehyde gas is condensed, furfural azeotrope with water object obtained in tower top,
First gold-plating bottom of towe discharge furfural.
Hydroxyl extracting method：Add pigment broken carboxyl compound plant, destroy plant cell wall, beta-glucosidase drop
Desugar is solved, hot alkaline water dissolving adds cationic surfactant combination reaction to stir, cooling, hydrochloric acid reaction reduction, freeze-drying
.
Embodiment 3
The present invention provides a kind of rare earth catching agent formula, the group ingredient including following weight percent：Hydroxyl 60%, naphthalene first
Acid 12%, formaldehyde 8%, furfural 18%, beauteously sub- orchid 2%, alkane kerosene 5%, the concentrated sulfuric acid 5%, sodium hydroxide 2%, hydrochloric acid hydroxyl
Amine 5%.
As a preferred technical solution of the present invention, preparation method is as follows：
Step 1：Hydroxyl, naphthoic acid and the concentrated sulfuric acid are pressed 2:1:1 ratio is added in three-necked flask, is sufficiently stirred 5 minutes,
Form it into yellow solution；
Step 2：By in solution of the concentrated sulfuric acid by a small amount of addition step 1 of dropping funel, 3 minutes are stood；
Step 3：The solution of step 2 is heated to reflux 24 hours, solution is made to react completely；
Step 4：The solution of step 3 is poured into beaker, is placed 8 hours, solution crystallization is complete；
Step 5：The crystallization of step 4 is filtered off into mother liquor, water washing is added to be dried at a temperature of 22 ° into neutrality；
Step 6：It will beauteously Ya Lan and alkane kerosene be put into agitator, and be stirred 10 minutes, poured into after stirring evenly
Flask；
Step 7：The crystallization of step 5 is put into reaction kettle, pure water is added in and is stirred 5 minutes；
Step 8：The flask contents of step 6 are poured into the reaction kettle of step 7, be stirred 5 minutes；
Step 9：Furfural and hydroxylamine hydrochloride are added in the reaction kettle of step 8,40 ° of heating is simultaneously reacted 5 hours, reaction knot
Beam postcooling is diluted with water to 24 °.
Furfural extracting method：Using bagasse as raw material, using dilute sulfuric acid catalyst, in hydrolytic process, steamed with high pressure water
Gas will hydrolyze the furfural generated and other by-product volatile materials take hydrolyzer out of, form aldehyde gas.Generally 4- containing furfural in aldehyde gas
6%, acetic acid 1_2%, also a small amount of low-boiling-point substance.Enter first gold-plating tower after aldehyde gas is condensed, furfural azeotrope with water object obtained in tower top,
First gold-plating bottom of towe discharge furfural.
Hydroxyl extracting method：Add pigment broken carboxyl compound plant, destroy plant cell wall, beta-glucosidase drop
Desugar is solved, hot alkaline water dissolving adds cationic surfactant combination reaction to stir, cooling, hydrochloric acid reaction reduction, freeze-drying
.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (7)
1. a kind of rare earth catching agent formula, it is characterised in that：Preparation method is as follows：
Step 1：Hydroxyl, naphthoic acid and the concentrated sulfuric acid are added in three-necked flask by a certain percentage, is sufficiently stirred 5~10 minutes, makes
It forms yellow solution；
Step 2：By the concentrated sulfuric acid by the solution described in a small amount of addition step 1 of dropping funel, standing 3~5 minutes；
Step 3：Solution described in step 2 is heated to reflux 24~48 hours, solution is made to react completely；
Step 4：Solution described in step 3 is poured into beaker, is placed 8~12 hours, solution crystallization is complete；
Step 5：Crystallization described in step 4 is filtered off into mother liquor, water washing is added to be dried at a temperature of 22 °~26 ° into neutrality；
Step 6：It will beauteously Ya Lan and alkane kerosene be put into agitator, and be stirred 10~15 minutes, poured into after stirring evenly
Flask；
Step 7：Crystallization described in step 5 is put into reaction kettle, pure water is added in and is stirred 5~10 minutes；
Step 8：Flask contents described in step 6 are poured into the reaction kettle described in step 7, are stirred 5~10 points
Clock；
Step 9：Furfural and hydroxylamine hydrochloride are added in the reaction kettle described in step 8,40 °~60 ° is heated and reaction 3~6 is small
When, it is cooled to 8 °~30 ° after reaction, is diluted with water.
2. a kind of rare earth catching agent formula according to claim 1, which is characterized in that include the group of following weight percent
Ingredient：Hydroxyl 40%~70%, naphthoic acid 10%~20%, formaldehyde 5%~10%, furfural 10%~20%, beauteously sub- orchid 2%
~10%, alkane kerosene 5%~10%, the concentrated sulfuric acid 5%~10%, sodium hydroxide 2%~10%, hydroxylamine hydrochloride 5%~15%.
3. a kind of rare earth catching agent formula according to claim 1, which is characterized in that the reaction kettle is reacted for enamel
Kettle.
4. a kind of rare earth catching agent formula according to claim 1-3, which is characterized in that the naphthoic acid, the formaldehyde,
The sodium hydroxide and the hydroxylamine hydrochloride are industrial rank.
A kind of 5. rare earth catching agent formula according to claim 1-4, which is characterized in that the furfural extracting method：With
Bagasse is raw material, and using dilute sulfuric acid catalyst, in hydrolytic process, the furfural and other generated will be hydrolyzed with high-pressure steam
By-product volatile materials takes hydrolyzer out of, forms aldehyde gas.Generally 4-6% containing furfural in aldehyde gas, acetic acid 1_2% are also a small amount of low
Boil object.Enter first gold-plating tower after aldehyde gas is condensed, obtain furfural azeotrope with water object in tower top, first gold-plating bottom of towe discharges furfural.
A kind of 6. rare earth catching agent formula according to claim 1, which is characterized in that the hydroxyl extracting method：By carboxylic
Based compound plant adds pigment broken, destroys plant cell wall, beta-glucosidase degradation desugar, and hot alkaline water dissolving adds sun
Ionic surface active agent combination reaction stirs, cooling, hydrochloric acid reaction reduction, freeze-drying.
7. a kind of rare earth catching agent formula according to claim 1, which is characterized in that the hydroxylamine hydrochloride nitrous acid is prepared
Method is as follows：Sodium synthetic method adds water to reaction kettle, is added with stirring sodium nitrite, adds in sodium pyrosulfite, Ran Houyong by several times
Sulfuric acid is acidified.Material after acidification is sent into hydrolysis kettle, acetone is added in, then neutralized with liquid caustic soda, neutralizer is distilled, obtains acetone
Oxime.It is reacted during acetoxime and hydrochloric acid are added in into salt oven, generates hydroxylamine hydrochloride and acetone.Acetone recycling uses；Hydroxylamine hydrochloride passes through
Concentration, crystallisation by cooling, centrifugation, drying are to get finished product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109395887A (en) * | 2018-12-11 | 2019-03-01 | 崔源发 | A kind of rare-earth ore ore-dressing method |
| CN111530633A (en) * | 2020-04-27 | 2020-08-14 | 西部矿业股份有限公司 | Novel composite collecting agent for recovering zinc oxide from peat plaza lead zinc oxide ore, preparation method and application |
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| CN101524670A (en) * | 2009-04-03 | 2009-09-09 | 包头市林峰稀土化工有限公司 | Rare earth collector |
| CN103240184A (en) * | 2013-05-17 | 2013-08-14 | 中国地质科学院矿产综合利用研究所 | Rare earth ore collecting agent, preparation method and mineral separation process of low-grade refractory rare earth ore |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109395887A (en) * | 2018-12-11 | 2019-03-01 | 崔源发 | A kind of rare-earth ore ore-dressing method |
| CN109395887B (en) * | 2018-12-11 | 2020-12-22 | 崔源发 | Rare earth ore dressing method |
| CN111530633A (en) * | 2020-04-27 | 2020-08-14 | 西部矿业股份有限公司 | Novel composite collecting agent for recovering zinc oxide from peat plaza lead zinc oxide ore, preparation method and application |
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