CN105669437A - Preparation method of nickel isooctanoate - Google Patents
Preparation method of nickel isooctanoate Download PDFInfo
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- CN105669437A CN105669437A CN201410678015.3A CN201410678015A CN105669437A CN 105669437 A CN105669437 A CN 105669437A CN 201410678015 A CN201410678015 A CN 201410678015A CN 105669437 A CN105669437 A CN 105669437A
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Abstract
The invention relates to a preparation method of nickel isooctanoate. An acidic eluent containing nickel is employed as a raw material. With effective combination of design of the reaction steps and parameter control, the nickel is recycled, environment pollution is reduced and cost is reduced. The preparation method is low in investment and cost. The added raw materials and solvents can be recycled. The method is suitable for industrial production and has very important practical significance.
Description
Technical field
The present invention relates to the preparation method of a kind of nickel iso-caprylate, more specifically relate to a kind of method utilizing the acidic effluent liquid containing nickel to prepare nickel iso-caprylate.
Background technology
Nickel iso-caprylate, English name Nickelisooctanoate, molecular formula: (C7H15COO)2Ni is a kind of green transparent thick liquid. The siccative being mainly used as coating, ink, catalyst for hydrogenation. Grinding distribution agent, ultraviolet absorbers etc. can also be done.
At present, produce nickel iso-caprylate and usually have following three kinds of methods. Method one: by metallic nickel and hydrochloric acid reaction, hydro-oxidation sodium, then add sulfuric acid temperature reaction, make nickel sulfate solution, then produce Sodium isooctanoate by isocaprylic acid and liquid caustic soda saponification, the finally obtained liquid nickel iso-caprylate with single nickel salt liquid and Sodium isooctanoate effect. Method two: by obtained to metallic nickel and nitric acid reaction nickelous nitrate, then generate Sodium isooctanoate by isocaprylic acid and liquid caustic soda saponification reaction, the finally obtained liquid nickel iso-caprylate with nickelous nitrate and Sodium isooctanoate effect. Method three: first generate nickel hydroxide with liquid caustic soda and nickelous nitrate effect, nickel hydroxide again with isocaprylic acid effect and obtained nickel iso-caprylate. Above three kinds of methods all make raw material with the compound of metallic nickel or nickel, but, the oxide compound market value of metallic nickel and nickel is expensive, and production cost height is low in economic efficiency. In above method, synthesis step is many simultaneously, and nickel receipts rate is low.
And in the prior art, containing the acidic effluent liquid of nickel, the nickel-containing waste water particularly produced in SEPS production process is owing to being difficult to recycle, general direct discharge, brings great hidden danger to like this improvement of environment.
Summary of the invention
It is an object of the invention to provide that a kind of technique is simple, nickel recovery height, can turn waste into wealth, reduce environmental pollution, less investment, the acidic effluent liquid containing nickel that utilizes that cost is low prepare the method for nickel iso-caprylate.
In order to realize foregoing invention object, the concrete technical scheme of the present invention is as follows:
A preparation method for nickel iso-caprylate, comprises the following steps: the pH value of the acidic effluent liquid containing nickel is adjusted to 3～4 by (1), adds aluminum precipitation agent, stirring reaction, filters, obtains aluminum precipitation and filtrate, the PH value of filtrate is adjusted to 1～3, the elutriant after being processed; (2) at 80～95 DEG C, isocaprylic acid and sodium hydroxide solution or potassium hydroxide solution mixing, carry out saponification reaction, obtain the product after isocaprylic acid saponification reaction; (3) at 80～95 DEG C, in the product after step (2) saponification reaction, the elutriant after the process adding step (1) is dripped, reaction; (4) being cooled to 60～75 DEG C, add organic solvent, stirring and dissolving, stratification, washing, collected organic layer, waste water is discharge after reclaiming nickel, and the nickel of recovery returns in step (1) and recycles;(5) by organic layer in-0.06～-0.09MPa, underpressure distillation at 60～90 DEG C, obtaining solvent and nickel iso-caprylate, solvent returns in step (4) and recycles;
Wherein, containing in the acidic effluent liquid of nickel, moisture 87～94 quality %, nickel 3～10 quality %, aluminium 0.008～0.25 quality %, hydrochloric acid 2～4 quality %, all the other are below 1 quality %;
Described aluminum precipitation agent is benzoate or ammoniacal liquor;
Described isocaprylic acid be 1:0.2～0.6 containing the mol ratio of nickel in the acidic effluent liquid of nickel;
Aluminum precipitation agent and be 1:0.2～0.4 containing the mol ratio of aluminium in the acidic effluent liquid of nickel.
Described isocaprylic acid is preferably 1:0.36～0.49 with containing the mol ratio of nickel in the acidic effluent liquid of nickel.
Described aluminum precipitation agent and mol ratio preferably 1:0.26～0.32 containing aluminium in the acidic effluent liquid of nickel.
The temperature of reaction of step (2) is preferably 90～92 DEG C.
The temperature of reaction of step (3) is preferably 85～92 DEG C.
Containing, in the acidic effluent liquid of nickel, the content of nickel is preferably 5-7 quality %.
By the optimization of above-mentioned parameter, it is possible to improve the rate of recovery of nickel further, obtain better economic benefit.
The described acidic effluent liquid containing nickel is preferably in SEPS production process the nickel-containing waste water produced.
Stirring reaction 0.5～2h in step (1); The time of the saponification reaction of step (2) is 1～2h; 0.5～2h is reacted after step (3) is dripped the elutriant after the process adding step (1).
In the saponification reaction of step (2), isocaprylic acid mixes according to mol ratio 1:0.8～0.95 with sodium hydroxide or potassium hydroxide.
Described benzoate is preferably Ammonium benzoate or Sodium Benzoate.
Described organic solvent is hexanaphthene or solvent oil.
The pH value of the acidic effluent liquid containing nickel is adjusted to 3～4 by adding alkaline matter by step (1).
Alkaline matter is preferably sodium hydroxide or sodium carbonate.
The PH value of filtrate is adjusted to 1～3, the preferred hydrochloric acid of mineral acid by adding mineral acid by step (1).
Sodium hydroxide solution or potassium hydroxide solution in step (2) are aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its concentration is 5-15 quality %.
Aqueous sodium hydroxide solution or potassium hydroxide aqueous solution are preferably 10%.
The useful effect of the present invention
The present invention is directed to the cost height of preparing nickel iso-caprylate in prior art, economic benefit low, and the discharge of nickel-containing waste water not only causes huge environmental stress, also result in the present situation of the loss of nickel resources, it is proposed that the present invention. The present invention prepares nickel iso-caprylate using the acidic effluent liquid containing nickel as raw material, by effective combination of the design of each reactions steps and state modulator, not only achieve the recycling of nickel, decrease environmental pollution, reduce cost, and technique of the present invention is simple, nickel recovery height. Preparing nickel iso-caprylate less investment, cost by the present invention low, the raw material added and solvent can recycle, and are applicable to suitability for industrialized production, have extremely important realistic meaning.
Embodiment
Hereinafter, " % " all represents " quality % ".
Embodiment 1
Acidic effluent liquid containing nickel: nickel content 3%, aluminium content 0.15%, hydrochloric acid 3%, water～94%.
(1) Feedstock treating: stir the pH to 3.5 that the lower NaOH solution with 10% regulates elutriant, be that 1:0.32 adds Ammonium benzoate by the mol ratio of aluminium in Ammonium benzoate and elutriant, react 1h under normal temperature, filter, collect filtrate, regulate PH=1 with hydrochloric acid, for subsequent use. In elutriant after process: nickel content is 3%, aluminium content is 0.0013%, water～97%.
(2) react: the NaOH solution 205g of 82g isocaprylic acid and 10% is joined in reactor, heating, stir, 2h is reacted at 90 DEG C, then, at 90 DEG C of temperature, slowly add the elutriant after 465g process, after reinforced, continue insulation reaction 1h, after having reacted, add 600g hexanaphthene, stirring and dissolving, stratification, divide phase of anhydrating, organic phase deionized water wash 2 times, divide phase of anhydrating, organic phase is at-0.06～-0.09MPa, underpressure distillation at 60～90 DEG C, desolvation and water, obtain nickel iso-caprylate 86g, nickel content 14.9%, nickel recovery 92.4%.
Embodiment 2
Except the mol ratio of the Ammonium benzoate in (1) and aluminium is 1:0.26, the method same according to embodiment 1 is reacted, and obtains nickel iso-caprylate 86.1g, nickel content 14.8%, nickel recovery 91.8%.
Embodiment 3
Except nickel content is 6%, the add-on of elutriant is 233g outer (keeping substantially identical with the total content of the nickel in embodiment 1), according to the method that embodiment 1 is same, obtains nickel iso-caprylate 94.3g, nickel content 14.3%, nickel recovery 97%.
Embodiment 4
Except nickel content is 10%, the add-on of elutriant is 140g outer (keeping substantially identical with the total content of the nickel in embodiment 1), according to the method that embodiment 1 is same, obtains nickel iso-caprylate 94g, nickel content 13.9%, nickel recovery 94%.
Embodiment 5
Except being changed to except ammoniacal liquor by the Ammonium benzoate in step (1), according to the method that embodiment 1 is same, obtain nickel iso-caprylate 84g, nickel content 14.3%, nickel recovery 86.4%.
Embodiment 6
Except in (2) step 10% NaOH be 190g except, the method same according to embodiment 1 is reacted, and obtains nickel iso-caprylate 80.3g, nickel content 13.9%, and nickel reclaims receipts rate 80.2%.
Embodiment 7
Except in (2) step 10% NaOH solution be 216g except, the method same according to embodiment 1 is reacted, and obtains nickel iso-caprylate 86.1g, nickel content 14%, nickel recovery 86.7%.
Embodiment 8
Except regulating PH=3 with hydrochloric acid, according to the method that embodiment 2 is same, obtain nickel iso-caprylate 87.1g, nickel content 14.7%, nickel recovery 92.1%.
Embodiment 9
Except heating in step (2), stir, at 95 DEG C, react 1h, then, at 90 DEG C, at this temperature, slowly add outside 465g elutriant, according to the method that embodiment 5 is same, obtain nickel iso-caprylate 82.3g, nickel content 14.1%, nickel recovery 83.5%,
Comparative example 1
Except step (1) regulates PH=5 with hydrochloric acid, according to the method that embodiment 1 is same, obtain nickel iso-caprylate 78g, nickel content 11.2%, nickel recovery 62.8%.
Comparative example 2
Except in step (2) at 97 DEG C of temperature, slowly add outside elutriant, according to the method that embodiment 1 is same, obtain nickel iso-caprylate 62g, nickel content 11.7%, nickel recovery 52.2%.
Comparative example 3
Except the add-on of elutriant in step (2) is 504g, according to the method that embodiment 1 is same, obtain nickel iso-caprylate 87.1g, nickel content 11.5%, nickel recovery 65.9%.
Claims (10)
1. a preparation method for nickel iso-caprylate, comprises the following steps: the pH value of the acidic effluent liquid containing nickel is adjusted to 3～4 by (1), adds aluminum precipitation agent, stirring reaction, filters, obtains aluminum precipitation and filtrate, the PH value of filtrate is adjusted to 1～3, the elutriant after being processed; (2) at 80～95 DEG C, isocaprylic acid and sodium hydroxide solution or potassium hydroxide solution mixing, carry out saponification reaction, obtain the product after isocaprylic acid saponification reaction;(3) at 80～95 DEG C, in the product after step (2) saponification reaction, the elutriant after the process adding step (1) is dripped, reaction; (4) being cooled to 60～75 DEG C, add organic solvent, stirring and dissolving, stratification, washing, collected organic layer, waste water is discharge after reclaiming nickel, and the nickel of recovery returns in step (1) and recycles; (5) by organic layer in-0.06～-0.09MPa, underpressure distillation at 60～90 DEG C, obtaining solvent and nickel iso-caprylate, solvent returns in step (4) and recycles;
Wherein, containing in the acidic effluent liquid of nickel, moisture 87～94 quality %, nickel 3～10 quality %, aluminium 0.008～0.25 quality %, hydrochloric acid 2～4 quality %, all the other are below 1 quality %;
Described aluminum precipitation agent is benzoate or ammoniacal liquor;
Described isocaprylic acid be 1:0.2～0.6 containing the mol ratio of nickel in the acidic effluent liquid of nickel;
Aluminum precipitation agent and be 1:0.2～0.4 containing the mol ratio of aluminium in the acidic effluent liquid of nickel.
2. preparation method according to claim 1, it is characterised in that, described isocaprylic acid be 1:0.36～0.49 containing the mol ratio of nickel in the acidic effluent liquid of nickel.
3. preparation method according to claim 1 and 2, it is characterised in that, described aluminum precipitation agent and be 1:0.26～0.32 containing the mol ratio of aluminium in the acidic effluent liquid of nickel.
4. preparation method according to claim 1, it is characterised in that, the temperature of reaction of step (2) is 90～92 DEG C.
5. preparation method according to claim 1 or 4, it is characterised in that, the temperature of reaction of step (3) is 85～92 DEG C.
6. preparation method according to claim 1, it is characterised in that, containing, in the acidic effluent liquid of nickel, the content of nickel is 5-7 quality %.
7. preparation method according to claim 1 or 6, it is characterised in that, the described acidic effluent liquid containing nickel is the nickel-containing waste water produced in SEPS production process.
8. preparation method according to claim 1, it is characterised in that, stirring reaction 0.5～2h in step (1); The time of the saponification reaction of step (2) is 1～2h; 0.5～2h is reacted after step (3) is dripped the elutriant after the process adding step (1).
9. preparation method according to claim 1, it is characterised in that, in the saponification reaction of step (2), isocaprylic acid and sodium hydroxide or potassium hydroxide mix according to mol ratio 1:0.8～0.95.
10. preparation method according to claim 1, it is characterised in that, described benzoate is Ammonium benzoate or Sodium Benzoate; Described organic solvent is hexanaphthene or solvent oil.
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Cited By (5)
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| CN106699545A (en) * | 2016-07-13 | 2017-05-24 | 广州新驰化工科技有限公司 | Preparation method of high-purity iron isooctoate |
| CN106757139A (en) * | 2016-12-12 | 2017-05-31 | 中南大学 | A kind of method of electrochemistry formated isooctyl acid slaine |
| CN107827736A (en) * | 2017-12-08 | 2018-03-23 | 成都蓉橙九天生物科技有限公司 | A kind of preparation method of cupric octoate and sad copper products |
| CN112851843A (en) * | 2021-01-11 | 2021-05-28 | 中国石油天然气股份有限公司锦州石化分公司 | Preparation and application of nickel-based catalyst for butadiene rubber polymerization |
| CN114195551A (en) * | 2021-11-20 | 2022-03-18 | 赣州科盈结构陶瓷有限公司 | Bill zirconia ceramic and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106699545A (en) * | 2016-07-13 | 2017-05-24 | 广州新驰化工科技有限公司 | Preparation method of high-purity iron isooctoate |
| CN106757139A (en) * | 2016-12-12 | 2017-05-31 | 中南大学 | A kind of method of electrochemistry formated isooctyl acid slaine |
| CN107827736A (en) * | 2017-12-08 | 2018-03-23 | 成都蓉橙九天生物科技有限公司 | A kind of preparation method of cupric octoate and sad copper products |
| CN112851843A (en) * | 2021-01-11 | 2021-05-28 | 中国石油天然气股份有限公司锦州石化分公司 | Preparation and application of nickel-based catalyst for butadiene rubber polymerization |
| CN114195551A (en) * | 2021-11-20 | 2022-03-18 | 赣州科盈结构陶瓷有限公司 | Bill zirconia ceramic and preparation method thereof |
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