CN201406394Y - Preparation system for nonylsalicyaldehyde oxime - Google Patents
Preparation system for nonylsalicyaldehyde oxime Download PDFInfo
- Publication number
- CN201406394Y CN201406394Y CN2009203031190U CN200920303119U CN201406394Y CN 201406394 Y CN201406394 Y CN 201406394Y CN 2009203031190 U CN2009203031190 U CN 2009203031190U CN 200920303119 U CN200920303119 U CN 200920303119U CN 201406394 Y CN201406394 Y CN 201406394Y
- Authority
- CN
- China
- Prior art keywords
- order reaction
- inlet pipeline
- outlet conduit
- reaction vessel
- pipeline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a preparation system for producing nonylsalicyaldehyde oxime by using copper extractant. Two raw material inlet pipelines, a chlorine gas inlet pipeline, a recycling pipeline and an outlet pipeline connected with a second-order reaction vessel are arranged on a first-order reaction vessel; an inlet pipeline and an outlet pipeline connected with a third-order reaction vessel are respectively arranged on the second-order reaction vessel; a recycling pipeline and an outlet pipeline connected with a fourth-order reaction vessel are arranged on the third-order reaction vessel, an outlet pipeline is arranged on the fourth-order reaction vessel and connected with a fifth-order reaction vessel, and an inlet pipeline and an outlet pipeline connected with a sixth-order reaction vessel are arranged on the fifth-order reaction vessel; and an outlet pipeline, a recycling pipeline and an inlet pipeline for dilute hydrochloric acid are arranged on the sixth-order reactionvessel. By adopting the preparation system, the condensation reaction and the oxidation-reduction reaction are performed to the utilized nonylphenol and paraformaldehyde under the action of magnesiummethoxide, and the nonylsalicyaldehyde is obtained after acidification; and the nonylsalicyaldehyde reacts with aqueous solution of hydroxy lamine hydrochloride and sodium hydroxide to obtain the nonylsalicyaldehyde oxime.
Description
Technical field
The utility model relates to a kind of preparation system of copper extractant raw materials for production nonyl salicylaldoxime of chemical field.
Background technology
Basis as electronic industry, information industry and household electric appliances, the printed electronic circuit board industry of one of heavy polluted industry shifts to China one after another over nearly 20 years, make the printed electronic circuit board industry of China be kept above 10% annual growth rate in recent years always, nearly 3000 families of enterprise that multiple scale is arranged at present, annual production reaches 200,000,000 square metres, annual consume smart copper more than 100,000 tons, total copper amount has constituted serious harm more than 50,000 tons to the water resources of surrounding area in the spent etching solution of output.(application number: 200510035207.3) technology that discloses a kind of utilization " extraction Song breaks the electroprecipitation copper of being pregnent " improves the production cost of circuit board plant with the recycling of the copper in the filter mud in Chinese invention patent application " circuit board plant copper filter mud utilizes and treatment process ".The copper extraction is a chemical reaction process, in this process, and the H in the extractant molecules
+Cupric ion with in the solution, pass through organic phase--aqueous phase interface exchanges.This exchange velocity of organic phase and water, change of direction (extraction or strip) and quantity depend on the concentration of cupric ion in the concentration, solution of extraction agent and the acidity of solution.Such as: when the pH value of solution value 1.5 when above, extraction agent discharges H
+Exchange with cupric ion, this exchange is called extraction.If the acidity of water is than higher, such as the acid that contains 180g/L, extraction at this moment just can discharge Cu
2+And replace H
+, this exchange is called " back extraction ".The chemical equation of its extraction and back extraction is as follows:
Extraction [2RH]
0+ [Cu
2++ SO
4 2-] → [R
2Cu]
0+ [2H
++ SO
4 2-]
Back extraction [R
2Cu]
0+ [2H
++ SO
4 2-] → [2RH]
0+ [Cu
2++ SO
4 2-]
The development of copper extractant is very active always in the world, has the following kind more than 30 of kind of commercial production at present, but really has the two big classes of having only of industrial use value: hydroxyl-ketoxime class and aldol oximes.The performance characteristics of hydroxyl-ketoxime kind of extractants is: splendid being separated property, and lower extraction loss does not promote the formation of throw out, and rate of extraction is slower, and extraction intensity is medium, and representative products has Lix841.The characteristics of aldol oximes extraction agent are: extremely strong collection copper ability, and rate of extraction is fast, collection copper recovery height, but back extraction difficulty, poor stability, representative products have Lix622, Lix622N, Lix64N, M5640, PT5050.
At the shortcoming of aldol oximes extraction agent back extraction difficulty, poor stability, providing a kind of is the copper extractant of initial feed with the nonyl salicylaldoxime, improves the back extraction performance and the chemical stability of copper extractant.But the equipment nonyl phenol transformation efficiency of producing the nonyl salicylaldoxime at present is low, and solvent for use can't recycling in the preparation process, and environment is caused very big influence.
The utility model content
The nonyl salicylaldoxime preparation system that the utility model purpose is to provide a kind of novel texture utilizes nonyl phenol under the effect of magnesium methylate, with Paraformaldehyde 96 generation condensation, redox reaction, can get the nonyl salicylic aldehyde again after acidifying; The reactant aqueous solution of nonyl salicylic aldehyde and oxammonium hydrochloride and sodium hydroxide can make the nonyl salicylaldoxime.
The technical scheme that realizes the utility model purpose is:
A kind of nonyl salicylaldoxime preparation system, comprise condenser and reactor, in described reactor, be provided with whipping appts, it is characterized in that: the first order reaction still is provided with two material inlet pipelines, chlorine inlet pipeline, recovery channel and outlet conduit, and described chlorine inlet pipeline and outlet conduit are provided with described condenser;
Described outlet conduit links to each other with the inlet pipeline of second order reaction still, is respectively arranged with toluene and hydrochloric acid inlet pipeline and outlet conduit on described second order reaction still;
The outlet conduit of described second order reaction still links to each other with the inlet pipeline of third order reaction still, and described third order reaction still is provided with recovery channel and outlet conduit, and this recovery channel is provided with described condenser;
The outlet conduit of described third order reaction still links to each other with the inlet pipeline of fourth-order reaction still, described fourth-order reaction still is provided with outlet conduit, described outlet conduit links to each other by the inlet pipeline of described condenser with the Pyatyi reactor, described Pyatyi reactor is provided with the inlet pipeline of sherwood oil inlet pipeline and oxammonium hydrochloride and sodium hydroxide mixed solution, described Pyatyi reactor is provided with outlet conduit, and described outlet conduit links to each other with the inlet pipeline of six order reaction stills;
Described six order reaction stills are provided with outlet conduit and recovery channel, and described recovery channel is provided with described condenser, also are provided with the inlet pipeline of dilute hydrochloric acid on described six order reaction stills.
The utility model compared with prior art has following advantage:
1. can with nonyl phenol under the effect of magnesium methylate,, after acidifying, can get the nonyl salicylic aldehyde again by this change system with Paraformaldehyde 96 generation condensation, redox reaction; The reactant aqueous solution of nonyl salicylic aldehyde and oxammonium hydrochloride and sodium hydroxide can make the nonyl salicylaldoxime.
This preparation system in use the nonyl phenol transformation efficiency up to 99%, nonyl salicylaldoxime recovery rate is up to 96%, and solvent for use all can recycling in the preparation process, and the rate of recovery all reaches more than 95%, can not cause big influence to environment, be applicable to big industrial production.
Description of drawings
Fig. 1 is the structural representation of a kind of nonyl salicylaldoxime preparation system described in the utility model
Embodiment
As can be seen from Figure 1, a kind of nonyl salicylaldoxime preparation system is achieved in that when producing the nonyl salicylaldoxime
1. the preparation of magnesium methylate
At first magnesium chips is added in batches and be warming up to 42--48 ℃ of reaction in the methanol solution, after methyl alcohol and magnesium chips reaction normally, logical cooling water control temperature distills out unnecessary methyl alcohol after methyl alcohol and magnesium chips react completely between 30～40 ℃, promptly get the magnesium methylate of white powder.
2. the preparation of nonyl phenol magnesium methylate
In magnesium methylate, add with the good nonyl phenol solution of dilution with toluene, be warming up to about 80 ℃ and reflux, when question response solution changes dark oil liquid into, distill out the azeotrope of methyl alcohol and toluene after, promptly get the nonyl phenol magnesium methylate.
3. the preparation of nonyl salicylic aldehyde
In the toluene solution of nonyl phenol magnesium methylate, add Paraformaldehyde 96 in batches, controlled temperature is 75--85 ℃, engler distillation does not go out the azeotrope of methyl alcohol and toluene, the control temperature is continued about 2 hours of 75--85 ℃ of insulation in the reinforced back of finishing of Paraformaldehyde 96, cooling, the hcl acidifying that adds is to neutral, remove water after, distilling off solvent toluene promptly gets the nonyl salicylic aldehyde.
4. the preparation of nonyl salicylaldoxime
After the sherwood oil that nonyl salicylic aldehyde and about tetraploid is long-pending mixes, the aqueous solution that adds oxammonium hydrochloride and sodium hydroxide, about 10 hours of 40 ℃ of left and right sides oximation reactions, remove excessive oxyammonia with dilute hydrochloric acid, wash feed liquid with water to neutral, the distilling off solvent sherwood oil promptly gets the nonyl salicylaldoxime, and the nonyl salicylaldoxime of gained is a light yellow viscous liquid.
Claims (1)
1. nonyl salicylaldoxime preparation system, comprise condenser and reactor, in described reactor, be provided with whipping appts, it is characterized in that: the first order reaction still is provided with two material inlet pipelines, chlorine inlet pipeline, recovery channel and outlet conduit, and described chlorine inlet pipeline and outlet conduit are provided with described condenser;
Described outlet conduit links to each other with the inlet pipeline of second order reaction still, is respectively arranged with toluene and hydrochloric acid inlet pipeline and outlet conduit on described second order reaction still;
The outlet conduit of described second order reaction still links to each other with the inlet pipeline of third order reaction still, and described third order reaction still is provided with recovery channel and outlet conduit, and this recovery channel is provided with described condenser;
The outlet conduit of described third order reaction still links to each other with the inlet pipeline of fourth-order reaction still, described fourth-order reaction still is provided with outlet conduit, described outlet conduit links to each other by the inlet pipeline of described condenser with the Pyatyi reactor, described Pyatyi reactor is provided with the inlet pipeline of sherwood oil inlet pipeline and oxammonium hydrochloride and sodium hydroxide mixed solution, described Pyatyi reactor is provided with outlet conduit, and described outlet conduit links to each other with the inlet pipeline of six order reaction stills;
Described six order reaction stills are provided with outlet conduit and recovery channel, and described recovery channel is provided with described condenser, also are provided with the inlet pipeline of dilute hydrochloric acid on described six order reaction stills.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009203031190U CN201406394Y (en) | 2009-05-13 | 2009-05-13 | Preparation system for nonylsalicyaldehyde oxime |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009203031190U CN201406394Y (en) | 2009-05-13 | 2009-05-13 | Preparation system for nonylsalicyaldehyde oxime |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201406394Y true CN201406394Y (en) | 2010-02-17 |
Family
ID=41677326
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009203031190U Expired - Fee Related CN201406394Y (en) | 2009-05-13 | 2009-05-13 | Preparation system for nonylsalicyaldehyde oxime |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201406394Y (en) |
-
2009
- 2009-05-13 CN CN2009203031190U patent/CN201406394Y/en not_active Expired - Fee Related
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101239904B (en) | Method for reclaiming and treating phenol and p-hydroxybenzoic acid in p-hydroxybenzoic acid technique waste water | |
| CN103243218B (en) | A kind of from containing extracting the method for molybdenum and the application of extraction agent molybdenum high-concentration acidic wastewater leach liquor | |
| CN101654305A (en) | Process for changing phenolic nitrate effluent into useful material by extracting, evaporating, crystallizing and coupling | |
| CN101445444A (en) | Method for recovering dilute acetic acid by extraction and azeotropic distillation | |
| CN102730894A (en) | Method for treating waste alkaline liquor produced in butanol and octanol production device | |
| CN105293454A (en) | Method for preparing dilute nitric acid, sponge tin and polymeric aluminum through spent tin-fading liquid | |
| CN104588049A (en) | Solid acid catalyst as well as preparation method and application of solid acid catalyst | |
| CN103740938A (en) | Method for recovering cobalt in cobalt carbonate production wastewater by saponification-free solvent extraction method | |
| CN101386912A (en) | Copper extractive agent | |
| CN103627442A (en) | Biodiesel catalysis preparing method by employing solid catalyst | |
| CN201406394Y (en) | Preparation system for nonylsalicyaldehyde oxime | |
| CN100519701C (en) | Crude oil demulsifying agent | |
| CN111777495B (en) | Method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene | |
| CN101550074B (en) | Catalytic synthesizing method of benzaldehyde | |
| CN102344390A (en) | Preparation system of nonyl salicylaldoxime | |
| CN103112876A (en) | Method for preparing potassium nitrate by utilizing nitric acid and potassium chloride | |
| CN201406391Y (en) | Preparation system for N-910 copper extractant | |
| CN103304838A (en) | Extraction method for recycling and reusing waste liquid from production of polyaniline by electrochemical process | |
| CN103319318A (en) | Recovering and recycling method of excessive methyl catechol in vanillin production process | |
| CN103130721B (en) | Ornidazole synthetic method | |
| CN102029171A (en) | Catalyst for synthesizing diphenylmethane and preparation method thereof | |
| CN101413067B (en) | Chemical extraction apparatus for metal gallium | |
| CN105503789A (en) | Method for catalytic conversion of xylose into furfural by use of montmorillonite-supported metal ion solid acid | |
| CN104098122B (en) | Technology for non-acidification synthesis of cuprous chloride from waste circuit board | |
| CN208279337U (en) | A kind of methanol-to-olefins sour water stripper |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100217 Termination date: 20120513 |