CN104607159A - Novel chelate fiber as well as preparation method and application thereof - Google Patents

Novel chelate fiber as well as preparation method and application thereof Download PDF

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CN104607159A
CN104607159A CN201510025740.5A CN201510025740A CN104607159A CN 104607159 A CN104607159 A CN 104607159A CN 201510025740 A CN201510025740 A CN 201510025740A CN 104607159 A CN104607159 A CN 104607159A
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acid
thiocarbamide
gold
sodium
fiber
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路建美
徐庆锋
顾培洋
王丽华
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Suzhou University
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Suzhou University
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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
    • 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
    • B01J20/28023Fibres or filaments
    • 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
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a novel chelate fiber as well as a preparation method and an application thereof. Specifically, the chelate fiber for adsorbing gold ions takes an acrylic fiber as a base body, and the base body is loaded with a sulfamide group and a poly-(dithiocarboxymethyl) amino group by the aid of a covalent bond. The acrylic fiber and polyamine (or an aqueous solution of the polyamine) have an amination reaction and then have a sulfamide reaction with carbon disulfide and a disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution of alkali sulfide, the reaction pH value is adjusted with a sodium dihydrogen phosphate-phosphoric acid solution, and the final product, namely, the chelate fiber is obtained. The chelate fiber can highly selectively enrich low-concentration precious metal ions in a waste liquid; the chelate fiber is high in gold absorbing speed and large in absorbing quantity; the gold cyanogen waste liquid can be continuously treated with the absorbing technology, and the chelate fiber can be reused.

Description

A kind of novel chelate fibre and its production and use
Technical field
The invention belongs to chelate fibre preparing technical field, be specifically related to a kind of novel chelate fibre, its preparation method, and in process containing the purposes in golden cyanogen waste liquid.
Background technology
Chelate fibre is a kind of can absorption and the ideal material of Footwall drift ion, and its outstanding advantage is: 1, chelate fibre has the features such as specific area is large, adsorption capacity is large, adsorption rate is fast; 2, be easy to elute from chelate fibre by the metal ion adsorbed, workload is much smaller than the situation using resin as adsorbent.
It is following several that research about chelate fibre mainly concentrates in the past based on acrylic fiber: I, chelating fiber containing amidoxime group, front yard of such as making pottery first waits people to utilize azanol and acrylic fiber to react to have prepared chelating fiber containing amidoxime group, this chelate fibre can the extensive metal ion such as absorbing copper, zinc and gold, but this chelate fibre is selective poor, and course of reaction is comparatively responsive to temperature, easy caking (see: Wu Zhichuan, Wang Xueqian, pottery front yard first etc., the preparation and property [J] of the acrylic fiber of chelated metal ions textile journal, 2004,25 (6): 36-37); In addition, the big equality people of woods also studied the absorption of this chelate fibre to gold ion, and shortcoming is the same (see the big equality of woods, containing chelating fiber containing amidoxime group absorption, reduction Au 3+research (I)---containing chelating fiber containing amidoxime group to Au 3+absorption behavior [J], sCI, 1993,14 (2): 283-286); II, semicarbazides chelate fibre, the people such as such as Gong Bo woods utilize semicarbazides and acrylic fiber to react to have prepared semicarbazides fiber, and this fiber can be used for metal ion such as absorption bismuth, vanadium etc., but the less stable of this fiber (see: Bolin Gong, Xueqiang Li, Fengrun Wang et. al., Synthesis of polyacrylacylaminourea chelating fiber and properties of concentration and separation of trace metal ions from samples [J], analytica Chimica Acta, 2001,427 (2): 287-291); III, amination fiber, if the people such as Young Gun Ko are at AlCl 3utilize polyethylene polyamine and acrylic fiber to react under catalysis and prepared amination fiber, this chelate fibre can extensive adsorbing metal ions, but poor selectivity, and adsorption capacity little (see Young Gun Ko, Ung Su Choi, Je Wan Woo, et. al.equilibrium adsorption model of anions onto a novel synthesized chelating fiber under various pHs and Fourier transform infrared study of these adsorptions [J] journal of Polymer Science Part B:Polymer Physics, 2004,42 (13): 2430 ~ 2440); IV, many (carboxymethyl) chemical fibre are tieed up, the people such as such as University Of Tianjin Zhang Wenqin utilize the acrylic fiber of chloroacetic alkaline solution and amination to react to have prepared many (carboxymethyl) chemical fibre and tie up, this chelate fibre can present very low concentration by adsorption of metal ions to sewage, but the adsorption capacity of this fiber is little, affect its use on a large scale (see: Chinese invention patent application CN101264438A); V, sulphamide chemical fibre are tieed up, such as U.S. patent Nos application US3821127 discloses and a kind ofly adopts vulcanized sodium etc. to react with acrylic fiber the sulphamide chemical fibre prepared to tie up, and this fiber can the noble metal such as ADSORPTION OF GOLD, but the adsorbance of this fiber is limited, and adsorption rate is slow, be unfavorable for using.
Therefore, needing one at present badly can selective absorption precious metal ion (especially gold ion), and the demand that adsorption capacity is large, adsorption rate is fast, reusable, preparation method is simple and easy to do novel chelate fibre meets the aspects such as daily production, scientific research.
Summary of the invention
First, for above-mentioned situation, the invention provides a kind of chelate fibre for ADSORPTION OF GOLD ion, described chelate fibre take acrylic fiber as matrix, with covalent supporting sulfonyl amine groups and many (two sulfo-carboxymethyls) amino group on described matrix, wherein in every gram of chelate fibre, the load capacity of sulfonyl amine groups is 1 ~ 6mmol, and the load capacity of many (two sulfo-carboxymethyls) amino group is 1 ~ 5mmol.
Secondly, present invention also offers the preparation method of above-mentioned chelate fibre, the method comprises the following steps:
1) according to the ratio of the polyaminated maceration extract of 1g acrylic fiber correspondence 25 ~ 75ml, acrylic fiber is positioned in polyaminated maceration extract, be constant temperature oscillation reaction 1 ~ 12h under the condition of 60 ~ 150 DEG C in temperature, after filtration, neutrality, drying is washed to, obtain polyaminated acrylic fiber, wherein: described polyaminated maceration extract is the aqueous solution of ethylenediamine, diethylenetriamine or triethylene tetramine, the percent by volume of solute is 15 ~ 85%;
2) according to the bath raio of 1:10 ~ 100, the polyaminated acrylic fiber obtained in step 1) is positioned in sulfonyl amination maceration extract, be constant temperature oscillation reaction 1 ~ 12h under the condition of 60 ~ 150 DEG C in temperature, after filtration, be washed to neutrality, dry, obtain the chelate fibre for ADSORPTION OF GOLD ion, wherein: described sulfonyl amination maceration extract is made up of following ingredients by weight: 2 parts of carbon disulfide, 2 parts of vulcanized sodium or potassium sulfide, 1 ~ 10 part of sodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution and 1 ~ 10 part of sodium dihydrogen phosphate-phosphate buffer, its pH value controls between 7.5 ~ 9.
Preferably, react according to the ratio of the polyaminated maceration extract of 1g acrylic fiber correspondence 40 ~ 60ml in step 1), temperature is 90 ~ 120 DEG C, and the time is 3h.
Preferably, in polyaminated maceration extract described in step 1), the percent by volume of solute is 20 ~ 50%.
Preferably, step 2) in react according to the bath raio of 1:80 ~ 95, temperature is 80 ~ 85 DEG C, and the time is 1 ~ 2h.
Preferably, step 2) described in the pH value of sulfonyl amination maceration extract control 8.5.
Finally, present invention also offers above-mentioned chelate fibre in process containing the purposes in golden cyanogen waste liquid.Specifically, described purposes includes, but is not limited to the cyanide produced also is reclaimed in the absorption of above-mentioned chelate fibre method containing the gold ion in golden cyanogen waste liquid, and it comprises the steps:
1) acid solution is added to containing in golden cyanogen waste liquid, obtain acidifying solution, hydrogen cyanide (HCN) is removed to air-blowing in acidifying solution by air pump, then make acidifying solution flow into the adsorption column being filled with above-mentioned chelate fibre to adsorb, thiocarbamide eluent is adopted to carry out wash-out after absorption, obtain high concentration gold liquid, and obtain elemental gold by electrolysis;
2) the low-concentration gold liquid obtained after making electrolysis flows back to adsorption column, again carries out adsorbing, wash-out and electrolysis;
3), after wash-out, adopt alkali lye drip washing adsorption column, obtain leacheate, and make leacheate flow back to cyaniding workshop, reclaim the cyanide residued in acidifying solution;
4) make the hydrogen cyanide removed flow into alkaline post to adsorb, and make the raffinate after absorption flow back to cyaniding workshop, reclaim residual cyanide.
Preferably, acid solution described in step 1) be selected from sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid any one, preferably sulfuric acid, more preferably dilute sulfuric acid.
Preferably; the eluent of thiocarbamide described in step 1) is in any one in acid thiocarbamide, thiosemicarbazides, phenylthiourea, vinylthiourea, o-xylene thiourea, meta-xylene thiocarbamide, paraxylene thiocarbamide, dinitrogen benzene thiocarbamide, alpha-naphthylthiourea, sulfo-ring phosphoryl thiocarbamide, 4-pyridine thiocarbamide, 4-methylthiosemicarbazone, guanidine radicals thiocarbamide, wherein used acid be selected from sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid any one.
Preferably, alkali lye described in step 3) is the aqueous solution of any one in NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, saleratus, potash, sodium hydrogen phosphate, dipotassium hydrogen phosphate, preferred weak solution.
Preferably, described in step 4), alkaline column filling has any one in NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, saleratus, potash, calcium oxide, calcium hydroxide, sodium hydrogen phosphate, dipotassium hydrogen phosphate.
Due to the utilization of technique scheme, the present invention compared with prior art has the following advantages:
(1) on acrylic fiber matrix, two sulfo-carboxymethyl anion are introduced by carbon disulfide, can contact faster with Jinyang ion, make this chelate fibre adsorption rate fast, just reach capacity adsorbance in the very short time, and adsorption rate is 5 ~ 10 times of known at present similar sorbing material;
(2) on matrix, introduce a large amount of sulfur amide groups by sulfonyl aminating reaction, make this chelate fibre saturated extent of adsorption reach 4mmol/g, single treatment just can make the solubility of gold be low to moderate below 50ppb;
(3) at present the research of same type of material all also rests on the stage of metal master solution, and chelate fibre of the present invention and absorbing process thereof can process continuously containing golden cyanogen waste liquid and can recovery of cyanide;
(4) the precious metal ion solution enrichment of low concentration can be become the precious metal ion solution of high concentration by chelate fibre of the present invention, and this chelate fibre does not only adsorb other ion precious metal ion absorption or adsorbance is very little, have higher selective;
(5) can thiocarbamide wash-out be passed through after chelate fibre ADSORPTION OF GOLD of the present invention, can reuse after alkali lye drip washing rare on a small quantity, reuse more than 100 times;
(6) preparation process of chelate fibre of the present invention is simple, and raw materials used is all conventional chemical products, and reaction condition is gentle, and absorbing process is simple to operate, is very convenient to industrialization.
Accompanying drawing explanation
Fig. 1 is the schematic arrangement of the chelate fibre in the present invention.
Fig. 2 is chelate fibre ADSORPTION OF GOLD ion in the present invention and the process chart of recovery of cyanide.
Detailed description of the invention
Below with reference to specific embodiment and accompanying drawing, the present invention is made further instructions.
Embodiment one: the preparation of chelate fibre and recycle.
Get 6 × 102(dawn/mm) acrylic fiber 0.50g, being positioned over 20ml volume solubility is in the ethylenediamine solution of 20%, at 90 DEG C constant temperature oscillation reaction 3h, after filtration, be washed to neutrality, drying, obtain polyaminated acrylic fiber 0.62g.
Get 14g vulcanized sodium, being dissolved in 15g(concentration is 1g/mL) in sodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution, add 14g carbon disulfide again, finally instilling 15g(concentration is 1g/mL) sodium dihydrogen phosphate-phosphate buffer, obtain sulfonyl amination maceration extract (pH value is 8.5).Be positioned over by above-mentioned polyaminated acrylic fiber in sulfonyl amination maceration extract, at 85 DEG C, constant temperature oscillation reaction 1h, after filtration, is washed to neutrality, drying, obtains many (two sulfo-carboxymethyls) amino fibre 0.95g of sulfonyl amination.
Products obtained therefrom is through nuclear magnetic resonance, infrared spectrum, elemental analysis, its structure as shown in Figure 1, wherein main chain is the matrix of acrylic fibers chelate fibre, with covalent supporting sulfonyl amine groups and many (two sulfo-carboxymethyls) amino group on it, in every gram of chelate fibre, the load capacity of sulfonyl amine groups is 1 ~ 6mmol, and the load capacity of many (two sulfo-carboxymethyls) amino group is 1 ~ 5mmol; Under different pH value condition, two sulfo-carboxymethyls can connect hydrogen ion, also can connect sodium ion, and there is dynamic equilibrium between sulfonyl amido and sulfydryl imino group (sulfo-amidino groups).
Above-mentioned fiber is positioned in fibre columns, measuring the gold concentration coming from certain factory is 1ppm(ICP-AES analysis-e/or determining, lower with) containing golden cyanogen waste liquid 5.10L, after the sulfuric acid acidation that 10ml volumetric concentration is 2%, air-blowing removes hydrogen cyanide, then flow into fibre columns to adsorb, with a small amount of acid thiourea wash-out after absorption, obtain the gold-containing solution (11ml) that concentration is 480ppm, golden simple substance is obtained by electrolysis, the rate of recovery 99% after solution enrichment.Above-mentioned fiber can Reusability after sodium acid carbonate drip washing rare on a small quantity.The hydrogen cyanide NaOH obtained absorbs, and can be reused in production, without the need to process.
Embodiment two: the preparation of chelate fibre and recycle.
Get 3 × 64(dawn/mm) acrylic fiber 0.50g, being positioned over 20ml volume solubility is in the diethylenetriamine aqueous solution of 30%, at 100 DEG C constant temperature oscillation reaction 3h, after filtration, be washed to neutrality, drying, obtain polyaminated acrylic fiber 0.65g.
Get 15g potassium sulfide, being dissolved in 15g(concentration is 1g/mL) in sodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution, adding 15g carbon disulfide, finally instilling 15g(concentration is 1g/mL) sodium dihydrogen phosphate-phosphate buffer, obtain sulfonyl amination maceration extract (pH value is 8.5).Be positioned over by above-mentioned polyaminated acrylic fiber in sulfonyl amination maceration extract, at 85 DEG C, constant temperature oscillation reaction 2h, after filtration, is washed to neutrality, drying, obtains many (two sulfo-carboxymethyls) amino fibre 0.96g of sulfonyl amination.
Above-mentioned fiber is positioned in fibre columns, measure the gold concentration coming from certain factory be 1ppm containing golden cyanogen waste liquid 5.50L, after the sulfuric acid acidation that 10ml volumetric concentration is 2%, air-blowing removes hydrogen cyanide, then flow into fibre columns to adsorb, with a small amount of acid amino wash-out after absorption, obtain the gold-containing solution (11ml) that concentration is 485ppm, obtain elemental gold by electrolysis after solution enrichment, the rate of recovery 99%.Above-mentioned fiber can Reusability after sodium acid carbonate drip washing rare on a small quantity.Obtain hydrogen cyanide sodium acid carbonate to absorb, can be reused in production, without the need to process.
Embodiment three: the preparation of chelate fibre and recycle.
Get 6 × 38(dawn/mm) acrylic fiber 0.50g, being positioned over 20ml volume solubility is in the triethylene tetramine aqueous solution of 30%, at 120 DEG C constant temperature oscillation reaction 3h, after filtration, be washed to neutrality, drying, obtain polyaminated acrylic fiber 0.68g.
Get 14g vulcanized sodium, being dissolved in 15g(concentration is 1g/mL) in sodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution, add 14g carbon disulfide again, finally instilling 15g(concentration is 1g/mL) sodium dihydrogen phosphate-phosphate buffer, obtain sulfonyl amination maceration extract (pH value is 8.5).Be positioned over by above-mentioned polyaminated acrylic fiber in sulfonyl amination maceration extract, at 80 DEG C, constant temperature oscillation reaction 2h, after filtration, is washed to neutrality, drying, obtains many (two sulfo-carboxymethyls) amino fibre 1.08g of sulfonyl amination.
Above-mentioned fiber is positioned in fibre columns, measure the gold concentration coming from certain factory be 1ppm containing golden cyanogen waste liquid 6.02L, after the sulfuric acid acidation that 10ml volumetric concentration is 2%, air-blowing removes hydrogen cyanide, then flow into fibre columns to adsorb, with a small amount of acid phenylthiourea wash-out after absorption, obtain the gold-containing solution (11ml) that concentration is 493ppm, obtain elemental gold by electrolysis after solution enrichment, the rate of recovery 99%.Above-mentioned fiber can Reusability after sodium acid carbonate drip washing rare on a small quantity.Obtain hydrogen cyanide NaOH to absorb, can be reused in production, without the need to process.
Embodiment four: the preparation of chelate fibre and recycle.
Get 1.5 × 64(dawn/mm) acrylic fiber 0.50g, being positioned over 30ml volume solubility is in the diethylenetriamine aqueous solution of 50%, at 100 DEG C constant temperature oscillation reaction 3h, after filtration, be washed to neutrality, drying, obtain polyaminated acrylic fiber 0.75g.
Get 15g potassium sulfide, being dissolved in 15g(concentration is 1g/mL) in sodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution, add 15g carbon disulfide again, then instilling 15g(concentration is 1g/mL) sodium dihydrogen phosphate-phosphate buffer, obtain sulfonyl amination maceration extract (pH value is 8.5).Be positioned over by above-mentioned polyaminated acrylic fiber in sulfonyl amination maceration extract, at 85 DEG C, constant temperature oscillation reaction 2h, after filtration, is washed to neutrality, drying, obtains many (two sulfo-carboxymethyls) amino fibre 1.08g of sulfonyl amination.
Above-mentioned fiber is positioned in fibre columns, measure the gold concentration coming from certain factory be 1ppm containing golden cyanogen waste liquid 5.50L, after the sulfuric acid acidation that 10ml volumetric concentration is 2%, air-blowing removes hydrogen cyanide, then flow into fibre columns to adsorb, with a small amount of acid thiourea wash-out after absorption, obtain the gold-containing solution (11ml) that concentration is 495ppm, obtain elemental gold by electrolysis after solution enrichment, the rate of recovery 99%.Above-mentioned fiber can Reusability after sodium acid carbonate drip washing rare on a small quantity.Obtain hydrogen cyanide sodium acid carbonate to absorb, can be reused in production, without the need to process.

Claims (9)

1. for a chelate fibre for ADSORPTION OF GOLD ion, described chelate fibre take acrylic fiber as matrix, with covalent supporting sulfonyl amine groups and many (two sulfo-carboxymethyls) amino group on described matrix;
Wherein: in every gram of chelate fibre, the load capacity of sulfonyl amine groups is 1 ~ 6mmol, the load capacity of many (two sulfo-carboxymethyls) amino groups is 1 ~ 5mmol.
2. a preparation method for the chelate fibre for ADSORPTION OF GOLD ion according to claim 1, it comprises the following steps:
1) according to the ratio of the polyaminated maceration extract of 1g acrylic fiber correspondence 25 ~ 75ml, acrylic fiber is positioned in polyaminated maceration extract, be constant temperature oscillation reaction 1 ~ 12h under the condition of 60 ~ 150 DEG C in temperature, after filtration, be washed to neutrality, drying, obtain polyaminated acrylic fiber;
Wherein: described polyaminated maceration extract is the aqueous solution of ethylenediamine, diethylenetriamine or triethylene tetramine, volume solubility is 15 ~ 85%;
2) according to the bath raio of 1:10 ~ 100, the polyaminated acrylic fiber obtained in step 1) is positioned in sulfonyl amination maceration extract, be constant temperature oscillation reaction 1 ~ 12h under the condition of 60 ~ 150 DEG C in temperature, after filtration, be washed to neutrality, drying, obtain the chelate fibre for ADSORPTION OF GOLD ion;
Wherein: described sulfonyl amination maceration extract is made up of following ingredients by weight: 2 parts of carbon disulfide, 2 parts of vulcanized sodium or potassium sulfide, 1 ~ 10 part of sodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution and 1 ~ 10 part of sodium dihydrogen phosphate-phosphate buffer, its pH value controls between 7.5 ~ 9.
3. the chelate fibre for ADSORPTION OF GOLD ion according to claim 1 contains the purposes in golden cyanogen waste liquid in process.
4. purposes according to claim 3, is characterized in that, described purposes is the cyanide produced also is reclaimed in chelate fibre absorption method containing the gold ion in golden cyanogen waste liquid, and it comprises the steps:
1) acid solution is added to containing in golden cyanogen waste liquid, obtain acidifying solution, hydrogen cyanide is removed to air-blowing in acidifying solution by air pump, then make acidifying solution flow into the adsorption column being filled with above-mentioned chelate fibre to adsorb, thiocarbamide eluent is adopted to carry out wash-out after absorption, obtain high concentration gold liquid, and obtain elemental gold by electrolysis;
2) the low-concentration gold liquid obtained after making electrolysis flows back to adsorption column, again carries out adsorbing, wash-out and electrolysis;
3), after wash-out, adopt alkali lye drip washing adsorption column, obtain leacheate, and make leacheate flow back to cyaniding workshop, reclaim the cyanide residued in acidifying solution;
4) make the hydrogen cyanide removed flow into alkaline post to adsorb, and make the raffinate after absorption flow back to cyaniding workshop, reclaim residual cyanide.
5. purposes according to claim 4, is characterized in that, acid solution described in step 1) be selected from sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid any one.
6. purposes according to claim 5, is characterized in that, acid solution described in step 1) is dilute sulfuric acid.
7. purposes according to claim 4; it is characterized in that; the eluent of thiocarbamide described in step 1) is in any one in acid thiocarbamide, thiosemicarbazides, phenylthiourea, vinylthiourea, o-xylene thiourea, meta-xylene thiocarbamide, paraxylene thiocarbamide, dinitrogen benzene thiocarbamide, alpha-naphthylthiourea, sulfo-ring phosphoryl thiocarbamide, 4-pyridine thiocarbamide, 4-methylthiosemicarbazone, guanidine radicals thiocarbamide, wherein used acid be selected from sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid any one.
8. purposes according to claim 4, is characterized in that, alkali lye described in step 3) is the aqueous solution of any one in NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, saleratus, potash, sodium hydrogen phosphate, dipotassium hydrogen phosphate.
9. purposes according to claim 4, it is characterized in that, alkaline column filling described in step 4) has any one in NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, saleratus, potash, calcium oxide, calcium hydroxide, sodium hydrogen phosphate, dipotassium hydrogen phosphate.
CN201510025740.5A 2015-01-19 2015-01-19 Novel chelate fiber as well as preparation method and application thereof Pending CN104607159A (en)

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CN106311182A (en) * 2016-10-18 2017-01-11 江苏理工学院 Preparation method and application of ultrafine chelated fibers
CN106861648A (en) * 2017-04-10 2017-06-20 华南师范大学 A kind of preparation method and product for vulcanizing chelate modified stalk fibre adsorbent
CN109052605A (en) * 2018-07-26 2018-12-21 雷晓琳 A kind of heavy metal chelating agent and preparation method thereof
CN110952321A (en) * 2019-10-22 2020-04-03 深圳市金纤环保材料有限公司 Preparation method of scale inhibition fiber material
RU2766500C1 (en) * 2018-07-27 2022-03-15 Дзе Проктер Энд Гэмбл Компани Method for washing fabrics using a water-soluble product with a single-use dose
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