CN106064081A - A kind of preparation method of nickel plating solution detin adsorbent - Google Patents

A kind of preparation method of nickel plating solution detin adsorbent Download PDF

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Publication number
CN106064081A
CN106064081A CN201610417202.5A CN201610417202A CN106064081A CN 106064081 A CN106064081 A CN 106064081A CN 201610417202 A CN201610417202 A CN 201610417202A CN 106064081 A CN106064081 A CN 106064081A
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Prior art keywords
adsorbent
plating solution
tin
nickel plating
preparation
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CN201610417202.5A
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Chinese (zh)
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王琪宇
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Individual
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Priority to CN201610417202.5A priority Critical patent/CN106064081A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/265Synthetic macromolecular compounds modified or post-treated polymers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016Particle form
    • B01J20/28021Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The present invention relates to the preparation method of a kind of nickel plating solution detin adsorbent, hydroxypropyl dextran microspheres carries out amination, add (dimethyl amine) tin trimethyl, double lauryl amines are aminating agent, can prepare adsorbent.

Description

A kind of preparation method of nickel plating solution detin adsorbent
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the preparation side of particularly a kind of nickel plating solution detin adsorbent Method.
Background technology
The fault being commonly encountered in nickel plating solution, such as: pin hole, pit, decortication, coarse, turn black, grow dim, striped and embrittlement etc., Except minority is owing to solution composition imbalance, operating condition exceed technological specification in addition to causing, often miscellaneous with plating solution Matter is relevant.Tin impurity is more sensitive to nickel plating solution, when concentration reaches certain value, may result in the low current density district of plating piece Coating turns black.In the case that metallic nickel price escalates, some enterprises before workpiece barrel plating bright nickel, first plate in tin copper Ashbury metal, then plates one layer of thin nickel again, thus reduces the purpose of electroplating cost.According to this procedure operation, a small amount of copper Carried people's nickel bath with tin impurity.The current potential calibration of copper, can deposit in coating quickly.Stannous ion can be with nickel plating light Some composition of bright dose and catabolite thereof generate complex compound, and electrode potential is more negative in addition, and electrodeposition rate is relatively slow, therefore, sub- Tin ion can retain the long period affects the performance of plating solution in the plating solution.
CN101956074A discloses a kind of method removing tin from zinc aqueous slkali, relates to a kind of alkali leaching-electrolysis raw Pan belongs to the removal technology of tin in Zinc powder process leachate.First it is Sn by Theil indices > the zinc aqueous slkali of 2~7g/L is heated to 70 ~100 DEG C, then under the conditions of stirring (200~700r/min), adding metal zinc (100~400 mesh), metal zinc presses zinc In aqueous slkali, 3~12 times (i.e. Zn: Sn=3~12: 1 mol ratios) of tin molar content add, and react 3~15h, stop stirring, take advantage of Heat filtering, in the filtrate that detection is filtrated to get, tin concentration is less than 0.05g/L, and direct power transmission is long-pending carries zinc, and filter residue is for containing 90~95% Thick tin, sells.The present invention has except advantages such as tin are thorough, method is easy, can eliminate tin to follow-up Zinc electrolysis by the present invention The serious harm that process causes, ensures that Zinc electrolysis process is smoothed out, also can obtain the thick tin by-product with high added value simultaneously Product.
CN105217759A discloses a kind of waste water and removes tin agent except tin agent and preparation method thereof, above-mentioned waste water, by comprising The component of following weight portion is made: alundum (Al2O3) 15-20 part, calcium aluminate 8-11 part, diatomite 5-8 part, basic magnesium carbonate 4-7 Part, ferrous sulfate 2-4 part, polyethylene 2-3 part, potassium fluorozirconate 2-4 part, borosilicic acid 1-3 part, hydroxypropul starch sodium phosphate 2-3 part With dimethyl diallyl ammonium chloride 1-2 part.Present invention also offers a kind of waste water except the preparation method of tin agent.
The method removing tin impurity reported in current document, complicated component, easily entrain new impurity, so needing to send out Bright a kind of novel sorbing material, improves the adsorption capacity to tin.
Content of the invention
For the deficiencies in the prior art, the invention provides the preparation method of a kind of nickel plating solution detin adsorbent.By hydroxyl Propyl group dextran microspheres carries out amination, adds (dimethyl amine) tin trimethyl, and double lauryl amines are aminating agent, can prepare absorption Agent.
The preparation method of a kind of nickel plating solution detin adsorbent, comprises the following steps:
Hydroxypropyl dextran microspheres methyl alcohol is made sweller, and consumption is the 200-500% of hydroxypropyl dextran microspheres weight (wt);At a temperature of 20-50 DEG C, adding the reaction of (dimethyl amine) tin trimethyl, consumption is hydroxypropyl dextran microspheres weight 1-10% (wt), add double lauryl amine, be the 100-200% (wt) of hydroxypropyl dextran microspheres weight, be incubated 5-15h, The adsorbent being applied to remove tin ion can be prepared.
Described hydroxypropyl dextran microspheres can use commercially available prod, as Xi'an Sunresin New Materials Co., Ltd. is raw The hydroxypropyl dextran microspheres product producing.
Described (dimethyl amine) tin trimethyl, double lauryl amines can use commercially available prod.
Beneficial effects of the present invention:
The present invention uses hydroxypropyl dextran microspheres with aldehyde functions, through (dimethyl amine) tin trimethyl, double dodecanes Base amine amination generates dextran amine, introduces tin element, can improve the absorption property to tin impurity, nickel plating solution on microballoon skeleton In tin ion concentration be smaller than 1mg/L.
Detailed description of the invention
Following example only further illustrate the present invention, are not to limit the scope of protection of the invention.
Embodiment 1
In 1000L reactor, add 100Kg hydroxypropyl dextran microspheres, add 300Kg methyl alcohol;At a temperature of 30 DEG C, add (dimethyl amine) tin trimethyl reacts, and consumption is 5Kg, adds the double lauryl amine of 150Kg, is incubated 8h, filters, dry numbering For SX-1.
Embodiment 2
In 1000L reactor, add 100Kg hydroxypropyl dextran microspheres, add 200Kg methyl alcohol;At a temperature of 20 DEG C, add (dimethyl amine) tin trimethyl reacts, and consumption is 1Kg, adds the double lauryl amine of 100Kg, is incubated 5h, filters, dry, product Numbered SX-2.
Embodiment 3
In 1000L reactor, add 100Kg hydroxypropyl dextran microspheres, add 500Kg methyl alcohol;At a temperature of 50 DEG C, add (dimethyl amine) tin trimethyl reacts, and consumption is 10Kg, adds 20Kg ferric trichloride, adds the double lauryl amine of 200Kg, insulation 15h, filters, and dries, and production code member is SX-3.
Comparative example 1
It is added without (dimethyl amine) tin trimethyl, the other the same as in Example 1.The numbered SX-4 of products obtained therefrom.
Comparative example 2
It is added without double lauryl amine, the other the same as in Example 1.The numbered SX-5 of products obtained therefrom.
Comparative example 3
It is added without double lauryl amine, (dimethyl amine) tin trimethyl, the other the same as in Example 1.The numbered SX-6 of products obtained therefrom.
Embodiment 4
Prepare nickel plating solution with AR: six hydration nickel sulfate 200g/L, Nickel dichloride hexahydrate 50 g/L, boric acid 45g/L, Regulate plating solution pH=4.7 with sodium carbonate liquor, backward plating solution adds stannous chloride, makes the mass concentration of stannous ion reach 150mg/L。
Accurately weigh each 5g of adsorbent that pretreated embodiment 1-3 and comparative example 1-3 prepare, be placed in 250mL tool plug In ground triangular flask, precision adds the nickel plating solution that people 100mL configures, and triangular flask at room temperature vibrates 5h, fully adsorbs After, to filter, detection calculates the tin ion concentration after absorption in nickel plating solution, is shown in Table 1:
Table 1: list after the separation material absorption that this patent prepares
Production code member Tin ion concentration mg/L in nickel plating solution after absorption
W-1 0.9
W-2 1.1
W-3 0.7
W-4 3.6
W-5 4.9
W-6 18.2
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.It any with the present invention is Basis, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, equivalent replaces Change or modification etc., be all covered by among protection scope of the present invention.

Claims (2)

1. the preparation method of a nickel plating solution detin adsorbent, it is characterised in that comprise the following steps:
Hydroxypropyl dextran microspheres methyl alcohol is made sweller, at a temperature of 20-50 DEG C, adds (dimethyl amine) tin trimethyl Reaction, consumption is the 1-10% (wt) of hydroxypropyl dextran microspheres weight, adds double lauryl amine, is that hydroxypropyl glucan is micro- The 100-200% (wt) of ball weight, is incubated 5-15h, can prepare the adsorbent being applied to remove the adsorbent of tin ion.
2. the preparation method of a kind of nickel plating solution detin adsorbent according to claim 1, it is characterised in that methyl alcohol actuating quantity is The 200-500% (wt) of hydroxypropyl dextran microspheres weight.
CN201610417202.5A 2016-06-13 2016-06-13 A kind of preparation method of nickel plating solution detin adsorbent Pending CN106064081A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101444756A (en) * 2008-12-17 2009-06-03 凯瑞化工有限责任公司 Styrene-series ion-exchange fiber applied to boron adsorption and preparation method thereof
CN102908998A (en) * 2012-11-09 2013-02-06 济南大学 Preparation method of xanthate macro-pore dextrangel adsorbent
CN103464117A (en) * 2013-09-26 2013-12-25 济南大学 Preparation method of ethanediamine based porous dextrangel adsorbent
CN104707574A (en) * 2015-03-23 2015-06-17 济南大学 Preparation of sephadex solid-supported brominated 1-propyl-3 methylimidazole adsorbent
CN104759255A (en) * 2014-01-02 2015-07-08 天津大学 Octyl dextran microspheres and preparation method and protein adsorption application thereof
CN105195099A (en) * 2015-09-21 2015-12-30 济南大学 Preparation method of beta-cyclodextrin modified macroporous amino glucan adsorbent

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101444756A (en) * 2008-12-17 2009-06-03 凯瑞化工有限责任公司 Styrene-series ion-exchange fiber applied to boron adsorption and preparation method thereof
CN102908998A (en) * 2012-11-09 2013-02-06 济南大学 Preparation method of xanthate macro-pore dextrangel adsorbent
CN103464117A (en) * 2013-09-26 2013-12-25 济南大学 Preparation method of ethanediamine based porous dextrangel adsorbent
CN104759255A (en) * 2014-01-02 2015-07-08 天津大学 Octyl dextran microspheres and preparation method and protein adsorption application thereof
CN104707574A (en) * 2015-03-23 2015-06-17 济南大学 Preparation of sephadex solid-supported brominated 1-propyl-3 methylimidazole adsorbent
CN105195099A (en) * 2015-09-21 2015-12-30 济南大学 Preparation method of beta-cyclodextrin modified macroporous amino glucan adsorbent

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Application publication date: 20161102