CN109810023A - A kind of liquid bigcatkin willow sodium alkyl hydroxamate of high-content and its preparation method and application - Google Patents
A kind of liquid bigcatkin willow sodium alkyl hydroxamate of high-content and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of high amount of liquid Salicyl Hydroximic Acid sodium, belong to mineral and smelt field of material preparation.Preparation method of the present invention is that salicylate, hydroxyl sulfate carry out hydroxyl oximation reaction in the solution comprising macromolecule emulsifier, alkali, is separated by solid-liquid separation after, obtains the liquid bigcatkin willow sodium alkyl hydroxamate；The macromolecule emulsifier is at least one of phenethyl phenol formaldehyde resin polyoxyethylene ether, alkyl phenol formaldehyde resin polyoxyethylene ether, alkylphenol-polyethenoxy polyethenoxy ether, triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer.The present invention also provides using liquid bigcatkin willow sodium alkyl hydroxamate made from the preparation method, in terms of Salicyl Hydroximic Acid, Salicyl Hydroximic Acid content is 22.9%-23.8%.The present invention has the characteristics that be not required to repeat acid adding and adds alkali, high without waste water, product utilization rate and content.
Description
Technical field
The invention belongs to floating agent fields, are related to a kind of liquid bigcatkin willow sodium alkyl hydroxamate.
Background technique
The hydroxyl oximido of Salicyl Hydroximic Acid contains N atom and O atom, they have lone pair electrons, belongs to weak electron donor, very
It is easy to form stable chelate with metal ion, along with the phenolic hydroxyl group on phenyl ring, can be played with hydroxyl oximido and cooperate with chelating
The effect of metal ion.Therefore, Salicyl Hydroximic Acid is a kind of selectivity chelating type collecting agent well, extensively should be in flotation tin
Stone, in the flotation of a variety of oxide ores such as ilmenite, bastnaesite and Nb-Ta mineral and rare earth.
Currently, Salicyl Hydroximic Acid production mainly carries out hydroxyl oximation reaction to gaultherolin by hydroxylamine hydrochloride and obtains.Hydroxyl
There are two types of methods for oximation reaction, and one is solvent using methanol as solvent, is distilled off after having reacted to obtain product (Ruiqin
Wang,14N Quadrupole Double Resonance in Some Substituted HydroxamicAcids, JACS,
1989, (1), 114-120).Such method solvent for use methanol is inflammable and explosive, and water can be also generated in reaction, needs the side of rectifying
Method carries out alcohol-water separation, increases production difficulty；Another kind is to take water as a solvent, and hydroxylamine hydrochloride is hydroxyl oximate reagent, and cream is added
Agent (Zhou Yulin, a kind of improvement production method of Salicyl Hydroximic Acid, CN101519365A), makes gaultherolin in water with micro-
Small emulsion droplets form occurs, and increases the contact area of azanol and gaultherolin, carries out hydroxyl oximation reaction quickly.Such
The product of method mainly occurs in the form of Salicyl Hydroximic Acid solid, generally requires the acidification after hydroxyl oximate, and
Using when then need plus alkali is deployed, be dissolved in it after aqueous solution and carry out floating operation again.Adding alkali-acid adding-plus alkali in this way
During, not only a large amount of acid of repeat consumption, alkali, also bring a large amount of waste water handling problem, and contain one in waste water
It is partially soluble in the Salicyl Hydroximic Acid of water, more increases the processing difficulty of waste water, becomes the problem of frustration enterprise.
Therefore, the form of expression of product is improved, wastewater flow rate is reduced, production economy is improved and has great importance.
Summary of the invention
The present invention is directed to overcome existing technological deficiency, it is therefore an objective to provide a kind of high-content, be not required to carry out in use process
Repeat acid adding, alkaline cleaning, the Salicyl Hydroximic Acid sodium liquid that can be used directly.
The present invention also provides a kind of liquid bigcatkin willow sodium alkyl hydroxamate as made from the preparation method.
The preparation method of existing Salicyl Hydroximic Acid is mostly synthesis Salicyl Hydroximic Acid solid, however Salicyl Hydroximic Acid solid
It in as flotation collector use process, needs first plus during alkali-acid adding-plus alkali, so not only repeat consumption is big
Acid, the alkali of amount, also bring a large amount of waste water handling problem, and are dissolved in the Salicyl Hydroximic Acid of water in waste water containing some, more
Increase the processing difficulty of waste water.To overcome technological deficiency existing for existing preparation method, the present inventor attempts to provide a kind of liquid
Body Salicyl Hydroximic Acid sodium (Salicyl Hydroximic Acid solution), however, providing liquid bigcatkin willow sodium alkyl hydroxamate is not the simple of physical form
During which transformation needs to overcome the effective solid content of solution low (referring to Salicyl Hydroximic Acid sodium effective content in solution product), long-term steady
Qualitative not high technical problem.To overcome these technical problems, the present inventor is had found, by numerous studies using sulfuric acid finally
Azanol cooperates the Promethean macromolecule emulsifier of the present inventor as raw material, can cooperate with to obtain that effective solid content is high, solution is uniform
The liquid bigcatkin willow sodium alkyl hydroxamate that property is good, long-time stability are high；Therefore the following technical schemes are provided:
A kind of preparation method of liquid bigcatkin willow sodium alkyl hydroxamate, salicylate, hydroxyl sulfate are including macromolecule emulsifier, alkali
Solution in carry out hydroxyl oximation reaction, be separated by solid-liquid separation after, obtain the liquid bigcatkin willow sodium alkyl hydroxamate.
In the present invention, by using hydroxyl sulfate as azanol raw material, cooperate macromolecule emulsifier of the present invention, into
Row hydroxyl oximation reaction is simply separated by solid-liquid separation after reaction, and the liquid bigcatkin willow hydroxyl that effective solid content is high, stability is good can be obtained
Oxime acid sodium.
Preferably, first by macromolecule emulsifier, salicylate and water stirring and emulsifying；Hydroxyl sulfate, dissolution is then added
Add alkali again afterwards, carries out hydroxyl oximation reaction；It is separated by solid-liquid separation again after reaction, obtains the liquid bigcatkin willow sodium alkyl hydroxamate.This
The innovative macromolecule emulsifier of salicylate and the present invention is emulsified in advance, obtains ultra-fine emulsion droplet by invention research discovery；
Then again with hydroxyl sulfate haptoreaction, used macromolecule emulsifier also can effectively prevent the precipitation of Salicyl Hydroximic Acid sodium, right
The precipitation influence of sodium sulphate is small, and then cooperates with and be further conducive to that high effective solid content and the better liquid bigcatkin willow of stability is made
Sodium alkyl hydroxamate.
Preferably, the macromolecule emulsifier is phenethyl phenol formaldehyde resin polyoxyethylene ether, alkylphenol formaldehyde tree
Rouge polyoxyethylene ether, alkylphenol-polyethenoxy polyethenoxy ether, triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer
At least one of.The study found that can further be cooperated with hydroxyl sulfate using the preferred macromolecule emulsifier, it can be into one
Step promotes the solid content in product, further promotes the stability of product.
Further preferably, the macromolecule emulsifier is phenethyl phenol formaldehyde resin polyoxyethylene ether and alkyl phenol polyoxy
At least one of ethylene polyethenoxy ether.The study found that can further be promoted to obtain using the preferred macromolecule emulsifier
Product solid content.
Preferably, the salicylate has 1 structure of formula:
In formula 1, R is the alkyl of C1~4.
The R is, for example, methyl, ethyl, propyl, 1- butyl, isopropyl etc..
In the present invention, the R is preferably methyl.It that is to say, the salicylate is preferably gaultherolin.
In the present invention, the ratio between salicylate and azanol, the temperature of reaction process during hydroxyl oximation reaction, pH
Equal Parameter Conditions can select existing conventional method, or can be according to theoretical implementation well-known to those skilled in the art.Example
Such as, guarantee that hydroxyl sulfate is suitably excessive, the speed etc. of alkali is added dropwise in suitable control.
Research is it has furthermore been found that the molar ratio of the salicylate, hydroxyl sulfate is preferably 1: 0.55-0.6.Cooperation is originally
The invention macromolecule emulsifier, controls under the preferred ratio, is more advantageous to hydroxyl oximation reaction, and then help to improve
Product yield.
Preferably, macromolecule emulsifier is the 1-1.5% of salicylate quality, a side under the preferred scope is controlled
Face can make the sufficiently ultra-fine emulsification of salicylate, and Salicyl Hydroximic Acid sodium solid on the other hand can be effectively prevent to be precipitated.
Preferably, the molar ratio of the alkali added and hydroxyl sulfate is 5.2-5.3: 1 during hydroxyl oximation reaction.Control exists
Under the preferred range, is conducive to hydroxyl oximation reaction and carries out completely.
Using gaultherolin as raw material, preferably, first reacting 3- at lower than 33 DEG C during hydroxyl oximation reaction
5 hours；It is warming up to 40 ± 2 DEG C again, the reaction was continued 2-3 hours.
Further preferably, it during hydroxyl oximation reaction, is first reacted 3-5 hours at 28-29 DEG C；It is warming up to 40 DEG C again, after
Continuous reaction 2-3 hours.Under the preferred stability contorting, the solid content and stability of product can be further promoted.
A kind of preferred preparation method of the present invention, specifically includes the following steps:
Step (1): macromolecule emulsifier, gaultherolin being added in reaction flask, are uniformly mixed, and water, stirring cream is added
Change；
Step (2): hydroxyl sulfate, stirring and dissolving is added；
Step (3): being added dropwise sodium hydroxide aqueous slkali, and temperature is controlled at 28-29 DEG C or so, and rear insulation reaction 3- is added dropwise
5 hours, then 40 DEG C are warming up to, it reacts 2-3 hours；
Step (4): filtering sodium sulfate salt obtains finished product.
The temperature of solution must be not higher than 33 DEG C when lye is added dropwise in the step (3), be easy to produce bigcatkin willow when the temperature is excessively high
Sour by-product.
The step (4) is step (3) directly filtering afterwards, without cooling.
The macromolecule emulsifier preferably uses phenethyl phenol formaldehyde resin polyoxyethylene ether, and alkylphenol-formaldehyde resin is poly-
Ethylene oxide ether, alkylphenol-polyethenoxy polyethenoxy ether, the classes such as triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer
Like emulsifier.The preferred macromolecule emulsifier has emulsifying capacity strong, and the gaultherolin emulsion droplet of formation is compared to normal
Rule low molecule emulsifier such as OP class emulsifier be formed by it is smaller, be conducive to generate Salicyl Hydroximic Acid and further with sodium hydroxide
Reaction generates Salicyl Hydroximic Acid sodium and is dissolved in water, forms uniform solution；And the preferred emulsifier can unexpectedly increase
The stability for adding product, effectively prevent product to decompose.In addition, cooperating institute of the present invention using the macromolecule emulsifier
The Collaborative Control of the hydroxyl sulfate and other parameters stated can further promote the purpose product content of liquid product obtained,
Additionally aid the long-time stability for further promoting liquid product.
The hydroxyl oximate reagent be industrial hydroxyl sulfate, the reagent compared to hydroxylamine hydrochloride have it is cheap,
Solubility is low at room temperature, adds common-ion effect, it is easier to be precipitated from solution.Sal glauberi is precipitated, energy when filtering
A large amount of water and inorganic salts are taken away, the raising of Salicyl Hydroximic Acid sodium effective content is conducive to；When with hydroxylamine hydrochloride, the chlorination of generation
Sodium solubility is big, and being easy to saltout is precipitated Salicyl Hydroximic Acid sodium in the form of paste, and when production is easy to block drain hole, is unfavorable for
Production is carried out continuously.
Sodium sulfate salt is directly filtered after step 3, without cooling.
The invention also discloses liquid bigcatkin willow sodium alkyl hydroxamates made from a kind of preparation method, in terms of Salicyl Hydroximic Acid,
22~24wt% of its content；Further preferably 22.9~23.8wt%.
Liquid bigcatkin willow sodium alkyl hydroxamate of the present invention is in uniform and stable lotion.By three months, half a year to product
Tracking, for hair typically now under storage condition, Salicyl Hydroximic Acid sodium ingredient does not have any variation, will not generate sodium salicylate or its
Remaining rearrangement product.
The present invention also provides the applications of the liquid bigcatkin willow sodium alkyl hydroxamate described in one kind, as collecting agent, applied to mineral
Flotation.In the present invention, directly using the liquid bigcatkin willow sodium alkyl hydroxamate as collecting agent, simplified, acidification is needed not move through, directly
It scoops out for mineral floating.
The mineral are any mineral aggregate that Salicyl Hydroximic Acid collecting can be used；Preferably cassiterite, ilmenite, bastnaesite
With a variety of oxide ores such as Nb-Ta mineral and Rare Earth Mine.
The utility model has the advantages that
1, the present invention is not required to ineffectually carry out acid adding, alkaline cleaning repeatedly using liquid bigcatkin willow sodium alkyl hydroxamate as final products,
Production cost has been saved, productive labor amount and time are reduced；
2, wastewater discharge is reduced, product utilization rate is improved.Waste water after acid adding contains a large amount of acid, inorganic salts, needs
The operations such as neutralization, desalination could outlet；The Salicyl Hydroximic Acid of generation has certain solubility in aqueous solution, need to its into
Row removing processing, for vast medium-sized and small enterprises, the processing of this partial organic substances is highly difficult.By product shape of the invention
Formula, product are directly used in flotation, do not generate production waste water, and Salicyl Hydroximic Acid sodium can be completely used for flotation production, effectively
Improve the utilization rate of product.
3, the effective content of product is high.After completion of the reaction, some solid sediment, after be proved to be sodium sulphate
Salt, the form that sodium sulphate is precipitated in aqueous solution is sal glauberi, after filtering, can take away part water and nothing in solution system
Machine salt improves the effective content of Salicyl Hydroximic Acid sodium.
4, the stability of product is good.By three months, tracking of the half a year to product, find in locating temperature and pH condition
Under, Salicyl Hydroximic Acid sodium ingredient does not have any variation, will not generate sodium salicylate or remaining rearrangement product.
Therefore, the present invention has simple process, and no wastewater treatment, product utilization rate and effective content are high, and client is facilitated to make
The characteristics of using.
Specific embodiment:
Embodiment 1
By 50 grams of gaultherolins and 0.6 gram of phenethyl phenol formaldehyde resin polyoxyethylene ether (Xingtai blue sky fine chemistry industry stock
Part Co., Ltd, agriculture breast 400#) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring and emulsifying.Sulfuric acid hydroxyl is added
29.6 grams of amine, after dissolution, it is added dropwise 95 grams of sodium hydroxide solution of 40%, when dropwise addition, controls reacting liquid temperature at 28-29 DEG C,
PH value is not more than 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, then heats to 40 DEG C, reacts 3 hours.Reaction
After, it is filtered to remove the salt of precipitation, obtains the solution of the Salicyl Hydroximic Acid sodium of clear, in terms of Salicyl Hydroximic Acid, bigcatkin willow
Hydroximic acid content is 23.5%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition by-products.
Embodiment 2
By 50 grams of gaultherolins and 0.7 gram of phenethyl phenol formaldehyde resin polyoxyethylene ether (Xingtai blue sky fine chemistry industry stock
Part Co., Ltd, agriculture breast 400#) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring and emulsifying.Sulfuric acid hydroxyl is added
29.6 grams of amine, after dissolution, it is added dropwise 95 grams of sodium hydroxide solution of 40%, when dropwise addition, controls reacting liquid temperature at 28-29 DEG C,
PH value is not more than 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, then heats to 40 DEG C, reacts 3 hours.Reaction
After, it is filtered to remove the salt of precipitation, obtains the solution of the Salicyl Hydroximic Acid sodium of clear, in terms of Salicyl Hydroximic Acid, bigcatkin willow
Hydroximic acid content is 23.4%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition by-products.
Embodiment 3
By 50 grams of gaultherolins and 0.6 gram of alkyl phenol formaldehyde resin polyoxyethylene ether (limited public affairs of Handan Xin Diya chemical industry
Department, Nongru-700 #) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring and emulsifying.29.6 grams of hydroxyl sulfate are added,
After dissolution, it is added dropwise 95 grams of sodium hydroxide solution of 40%, when dropwise addition controls reacting liquid temperature at 28-29 DEG C, and pH value is little
In 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, 40 DEG C is then heated to, is reacted 3 hours.After completion of the reaction, mistake
The salt being precipitated is filtered out, the solution of the Salicyl Hydroximic Acid sodium of clear, in terms of Salicyl Hydroximic Acid, Salicyl Hydroximic Acid content are obtained
It is 22.9%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition by-products.
Embodiment 4
By 50 grams of gaultherolins and 0.7 gram of alkyl phenol formaldehyde resin polyoxyethylene ether (limited public affairs of Handan Xin Diya chemical industry
Department, Nongru-700 #) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring and emulsifying.29.6 grams of hydroxyl sulfate are added,
After dissolution, it is added dropwise 95 grams of sodium hydroxide solution of 40%, when dropwise addition controls reacting liquid temperature at 28-29 DEG C, and pH value is little
In 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, 40 DEG C is then heated to, is reacted 3 hours.After completion of the reaction, mistake
The salt being precipitated is filtered out, the solution of the Salicyl Hydroximic Acid sodium of clear, in terms of Salicyl Hydroximic Acid, Salicyl Hydroximic Acid content are obtained
It is 23.0%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition by-products.
Embodiment 5
By 50 grams of gaultherolins and 0.6 gram of alkylphenol-polyethenoxy polyethenoxy ether (the green gloomy chemical industry in Linyi, APEP-
108) it is added in three-necked flask, stirs evenly, be added 55 grams of water, stirring and emulsifying.29.6 grams of hydroxyl sulfate are added, dissolution finishes
Afterwards, 95 grams of sodium hydroxide solution of 40% are added dropwise, for control reacting liquid temperature at 28-29 DEG C, pH value is not more than 12, is added dropwise when dropwise addition
After (1.5 hours), insulation reaction 3 hours, then heat to 40 DEG C, react 3 hours.After completion of the reaction, it is filtered to remove analysis
Salt out obtains the solution of the Salicyl Hydroximic Acid sodium of clear, and in terms of Salicyl Hydroximic Acid, Salicyl Hydroximic Acid content is
23.8%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition by-products.
Embodiment 6
By 50 grams of gaultherolins and 0.7 gram of alkylphenol-polyethenoxy polyethenoxy ether (the green gloomy chemical industry in Linyi, APEP-
108) it is added in three-necked flask, stirs evenly, be added 55 grams of water, stirring and emulsifying.29.6 grams of hydroxyl sulfate are added, dissolution finishes
Afterwards, 95 grams of sodium hydroxide solution of 40% are added dropwise, for control reacting liquid temperature at 28-29 DEG C, pH value is not more than 12, is added dropwise when dropwise addition
After (1.5 hours), insulation reaction 3 hours, then heat to 40 DEG C, react 3 hours.After completion of the reaction, it is filtered to remove analysis
Salt out obtains the solution of the Salicyl Hydroximic Acid sodium of clear, and in terms of Salicyl Hydroximic Acid, Salicyl Hydroximic Acid content is
23.8%.It is tracked by 6 months gas-chromatographies, product stability is good, no decomposition by-products.
Embodiment 7
By 50 grams of gaultherolins and 0.6 gram of triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer, (Xingtai is blue
Its fine chemistry industry limited liability company, agriculture breast 1602#) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring cream
Change.29.6 grams of hydroxyl sulfate, after dissolution are added, is added dropwise 95 grams of sodium hydroxide solution of 40%, when dropwise addition controls reaction solution
For temperature at 28-29 DEG C, pH value is not more than 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, then heats to 40 DEG C,
Reaction 3 hours.After completion of the reaction, it is filtered to remove the salt of precipitation, the solution of the Salicyl Hydroximic Acid sodium of clear is obtained, with bigcatkin willow
Hydroximic acid meter, Salicyl Hydroximic Acid content are 23.2%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition
By-product.
Embodiment 8
By 50 grams of gaultherolins and 0.7 gram of triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer, (Xingtai is blue
Its fine chemistry industry limited liability company, agriculture breast 1602#) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring cream
Change.29.6 grams of hydroxyl sulfate, after dissolution are added, is added dropwise 95 grams of sodium hydroxide solution of 40%, when dropwise addition controls reaction solution
For temperature at 28-29 DEG C, pH value is not more than 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, then heats to 40 DEG C,
Reaction 3 hours.After completion of the reaction, it is filtered to remove the salt of precipitation, the solution of the Salicyl Hydroximic Acid sodium of clear is obtained, with bigcatkin willow
Hydroximic acid meter, Salicyl Hydroximic Acid content are 23.1%.Product is tracked with gas-chromatography, and product stability is good in 6 months, no decomposition
By-product.
Comparative example 1
By 50 grams of gaultherolins and 0.7 gram of nonylphenol polyoxyethylene ether (Xingtai blue sky fine chemistry industry limited liability company,
OP-10 it) is added in three-necked flask, stirs evenly, be added 55 grams of water, stirring and emulsifying.29.6 grams of hydroxyl sulfate are added, has been dissolved
Bi Hou, is added dropwise 95 grams of sodium hydroxide solution of 40%, and control reacting liquid temperature is at 28-29 DEG C when dropwise addition, and pH value is not more than 12, drop
After adding (1.5 hours), insulation reaction 3 hours, 40 DEG C are then heated to, is reacted 3 hours.After completion of the reaction, what is obtained is
A kind of solidliquid mixture includes a large amount of Salicyl Hydroximic Acid sodium in solid salt, is filtered to remove the salt of precipitation, in terms of Salicyl Hydroximic Acid,
Salicyl Hydroximic Acid content is 17.1% in solution.It is tracked with gas-chromatography, discovery has 10% product to be converted into bigcatkin willow after 6 months
Sour sodium.
Comparative example 2
By 50 grams of gaultherolins and 0.6 gram of phenethyl phenol formaldehyde resin polyoxyethylene ether (Xingtai blue sky fine chemistry industry stock
Part Co., Ltd, agriculture breast 400#) it is added in three-necked flask, it stirs evenly, is added 55 grams of water, stirring and emulsifying.Hydrochloric acid hydroxyl is added
25 grams of amine, after dissolution, it is added dropwise 95 grams of sodium hydroxide solution of 40%, control reacting liquid temperature is at 28-29 DEG C when dropwise addition, PH
Value is not more than 12, after being added dropwise (1.5 hours), insulation reaction 3 hours, then heats to 40 DEG C, reacts 3 hours.It has reacted
Bi Hou, what is obtained is a kind of solidliquid mixture, includes a large amount of Salicyl Hydroximic Acid sodium in solid salt, is filtered to remove the salt of precipitation, with
Salicyl Hydroximic Acid meter, Salicyl Hydroximic Acid content is 16.5% in solution.Product is tracked with gas-chromatography, and product is stablized in 6 months
Property is good, does not find decomposition by-products.
Claims (10)
1. a kind of preparation method of liquid bigcatkin willow sodium alkyl hydroxamate, which is characterized in that salicylate, hydroxyl sulfate are including macromolecule
Emulsifier, alkali solution in carry out hydroxyl oximation reaction, be separated by solid-liquid separation after, obtain the liquid bigcatkin willow sodium alkyl hydroxamate.
2. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as described in claim 1, which is characterized in that first by macromolecule emulsion
Agent, salicylate and water stirring and emulsifying；Hydroxyl sulfate is then added, adds alkali after dissolution again, carries out hydroxyl oximation reaction；Reaction terminates
It is separated by solid-liquid separation again afterwards, obtains the liquid bigcatkin willow sodium alkyl hydroxamate.
3. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 1 or 2, which is characterized in that the macromolecule
Emulsifier is phenethyl phenol formaldehyde resin polyoxyethylene ether, alkyl phenol formaldehyde resin polyoxyethylene ether, alkylphenol-polyethenoxy are poly-
At least one of oxypropylene ether, triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer.
4. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 1 or 2, which is characterized in that the salicylic acid
Ester has 1 structure of formula:
In formula 1, R is the alkyl of C1~4；Preferably methyl.
5. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 3, which is characterized in that the salicylate,
The molar ratio 1: 0.55-0.6 of hydroxyl sulfate.
6. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 3, which is characterized in that macromolecule emulsifier is water
The 1-1.5% of poplar acid esters quality.
7. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 3, which is characterized in that the alkali and sulfuric acid hydroxyl added
The molar ratio of amine is 5.2-5.3: 1.
8. the preparation method of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 3, which is characterized in that hydroxyl oximation reaction process
In, first reacted 3-5 hours at lower than 33 DEG C；It is warming up to 40 ± 2 DEG C again, the reaction was continued 2-3 hours.
9. liquid bigcatkin willow sodium alkyl hydroxamate made from a kind of any one of claim 1~8 preparation method, which is characterized in that with
Salicyl Hydroximic Acid meter, content are 22~24wt%.
10. a kind of application of liquid bigcatkin willow sodium alkyl hydroxamate as claimed in claim 9, which is characterized in that as collecting agent, be applied to
Mineral floating.
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| Title |
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| AUDREY BEILLARD，等: "A facile and rapid preparation of hydroxamic acids by hydroxylaminolysis using DBU as base", 《TETRAHEDRON LETTERS》 * |
| 符剑刚，等: "羟胺法合成羟肟酸的研究进展", 《广东有色金属学报》 * |
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|---|---|
| CN109810023B (en) | 2022-02-08 |
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