CN105833854A - Preparation method of purified vanadium adsorption material - Google Patents

Preparation method of purified vanadium adsorption material Download PDF

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Publication number
CN105833854A
CN105833854A CN201610408025.4A CN201610408025A CN105833854A CN 105833854 A CN105833854 A CN 105833854A CN 201610408025 A CN201610408025 A CN 201610408025A CN 105833854 A CN105833854 A CN 105833854A
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preparation
vanadium
oil
porogen
phase
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王琪宇
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
    • C08F222/02—Acids; Metal salts or ammonium salts thereof, e.g. maleic acid or itaconic acid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
    • C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F232/00—Copolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system
    • C08F232/08—Copolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having condensed rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
    • C08F259/02—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing chlorine
    • C08F259/06—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing chlorine on to polymers of vinylidene chloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Analytical Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention relates to a preparation method of a purified vanadium adsorption material. Bis(cyclopentadiene) vanadium iodide and octadecendioic acid are introduced in the polymerization process; 1-allyl-3-buthylimidazole tetrafluoroborate is used for polymerization and preparation.

Description

A kind of preparation purifying vanadium adsorbing material
Technical field
The present invention relates to the preparation of a kind of adsorbent, a kind of preparation purifying vanadium adsorbing material.
Background technology
During vanadium bearing slag leaches vanadium extraction, some impurity leach in solution together also with vanadium, leach containing vanadium Liquid usually contains the foreign ions such as ferrum, manganese, chromium, silicon, phosphorus, aluminum, calcium, has influence on the quality of precipitation and product, these impurity from Son under the adjustment of pH of leaching solution, major part foreign ion generation hydrolysis and precipitate entrance precipitation slag in, but, phosphorus, Still generate soluble compound after silicon, calcium and aluminum hydrolysis and stay in leachate, badly influence precipitation and product quality, it is necessary to remove To the greatest extent.So that special purified treatment, conventional minimizing technology generally has solvent extraction or ion exchange, but removal effect is equal Undesirable, therefore, how foreign matter of phosphor, silicon, calcium and aluminum are removed from vanadium-contained clinker leaching liquor, to meet wanting of product quality Ask and have very important significance.
CN103014377A discloses the method for purification of a kind of vanadium liquid, this vanadium liquid contain vanadic acid radical ion, silicate ion, Aluminium ion and calcium ion, the method comprises the following steps: vanadium liquid is contacted by (1) with cleaner A and cleaner B, so that vanadium Silicate ion in liquid forms precipitation with cleaner A, makes the aluminium ion in vanadium liquid and calcium ion form precipitation with cleaner B.
Disclosing a kind of method purifying vanadic anhydride in CN104843789A, described method comprises the steps: (1) Vanadium original solution calcification will be contained, be filtrated to get calcium vanadate solid phase；Afterwards the acidifying of calcium vanadate solid phase is obtained pending containing vanadium solution； (2) add cleaner and carry out remove impurity, be purified vanadium liquid and remove impurity mud；Described cleaner includes ammonium carbonate and/or ammonium hydrogen carbonate； (3) regulation purifies vanadium liquid pH value, adds (NH4)2SO4Carry out precipitation, obtain ammonium poly-vanadate precipitation, afterwards through adding heat extraction water And ammonia, obtain vanadic anhydride；Optional before or after step (1) carry out step (1): except silicon phosphorus impurities.
The method purifying vanadium reported in document at present, complicated component, process route is long, easily entrains new impurity, Directly vanadium being extracted from solution so needing to invent a kind of novel adsorbing material, improving the absorbability to vanadium.
Summary of the invention
For from containing the requirement extracting vanadium ion in vanadium solution, it is provided that a kind of preparation purifying vanadium adsorbing material, by with Lower step realizes:
The preparation of step 1. aqueous phase
By weight, 100 parts of pure water 0.5-2 part polyvinyl alcohol of interior addition, stir in a kettle.；
The preparation of step 2. oil phase
By weight, by 100 parts of vinylidene chlorides, 50-90 part double (cyclopentadiene) iodate vanadium, 20-50 part octadecene diacid, 0.1-0.5 part 1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate mixes, and adds 0.5-3 part benzoyl peroxide, 20-40 part Porogen, stirs；
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 10-24 at 80-110 DEG C H, reaction terminates rear blowing, by clean for porogen extracting after drying, obtains product.
Double (cyclopentadiene) iodate vanadium described in step 2, octadecene diacid is commercially available prod.
1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate described in step 2 is commercially available prod, such as Chinese Academy of Sciences's Lanzhou chemicals The product of reason Research Institute.
Porogen described in step 2 is good solvent or poor solvent or mixed solvent, such as white oil, and solvent naphtha, toluene etc., excellent Select toluene.
Beneficial effects of the present invention:
The present invention introduces double (cyclopentadiene) iodate vanadium in polymerization and combines with the pattern of chemical bond as comonomer, vanadium ion In the skeleton of resin, not easily run off, the absorbability of vanadium ion can be improved；Octadecene diacid, 1-pi-allyl-3-butyl miaow The addition of azoles tetrafluoroborate also gives the adsorbent more high absorption capacity to stannum.
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
The preparation of step 1. aqueous phase
By weight, in reactor, add 100 parts of pure water, 0.5 part of polyvinyl alcohol, stir.
The preparation of step 2. oil phase
By the oil phase component mixing and stirring of following ratio；
Ingredients weight parts
Vinylidene chloride 100
Double (cyclopentadiene) iodate vanadium 65
Octadecene diacid 33
1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.3
Toluene 30
Benzoyl peroxide 2
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 2 in step 1, equipped with in the reactor preparing aqueous phase, react 14h at 90 DEG C, Reaction terminates rear blowing, by clean for toluene extracting after drying, obtains product.Numbered W-1.
Embodiment 2
The preparation of step 1. aqueous phase
By weight, in reactor, add 100 parts of pure water, 1.5 parts of polyvinyl alcohol, stir.
The preparation of step 2. oil phase
By the oil phase component mixing and stirring of following ratio；
Ingredients weight parts
Vinylidene chloride 100
Double (cyclopentadiene) iodate vanadium 50
Octadecene diacid 20
1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.1
White oil 40
Benzoyl peroxide 0.5
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 24h, reaction knot at 80 DEG C Blowing after bundle, by clean for porogen extracting after drying, obtains product, numbered W-2.
Embodiment 3
The preparation of step 1. aqueous phase
By weight, in reactor, add 100 parts of pure water, 2 parts of polyvinyl alcohol, stir.
The preparation of step 2. oil phase
By the oil phase component mixing and stirring of following ratio；
Ingredients weight parts
Vinylidene chloride 100
Double (cyclopentadiene) iodate vanadium 90
Octadecene diacid 50
1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.5
Solvent naphtha 20
Benzoyl peroxide 3
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 10h, reaction knot at 110 DEG C Blowing after bundle, by clean for porogen extracting after drying, obtains product, numbered W-3.
Comparative example 1
It is added without octadecene diacid, the other the same as in Example 1.The numbered W-4 of products obtained therefrom.
Comparative example 2
It is added without 1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate, the other the same as in Example 1.The numbered W-5 of products obtained therefrom.
Comparative example 2
It is added without double (cyclopentadiene) iodate vanadium, the other the same as in Example 1.The numbered W-6 of products obtained therefrom.
Embodiment 4
Accurately weigh each 5g of adsorbent that pretreated embodiment 1-3 and comparative example 1-3 prepare, be placed in 250mL tool plug ground In triangular flask, precision adds the vanadic anhydride solution of people's 100mL concentration 150mg/L, and at room temperature vibrate 5h by triangular flask, fully After absorption, filtering, detection calculates the vanadic anhydride ion concentration after absorption in solution, is shown in Table 1:
Table 1: catalog after the separation material absorption that this patent prepares
Production code member Vanadic anhydride concentration mg/L in solution after absorption
W-1 4
W-2 6
W-3 3
W-4 11
W-5 16
W-6 78
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with the present invention it is Basis, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, equivalent are replaced Change or modification etc., be all covered by among protection scope of the present invention.

Claims (2)

1. purifying a preparation for vanadium adsorbing material, its feature its preparation method is to comprise the following steps:
The preparation of step 1. aqueous phase
By weight, 100 parts of pure water 0.5-2 part polyvinyl alcohol of interior addition, stir in a kettle.；
The preparation of step 2. oil phase
By weight, by 100 parts of vinylidene chlorides, 50-90 part double (cyclopentadiene) iodate vanadium, 20-50 part octadecene diacid, 0.1-0.5 part 1-pi-allyl-3-1-Butyl-1H-imidazole tetrafluoroborate mixes, and adds 0.5-3 part benzoyl peroxide, 20-40 part Porogen, stirs；
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 10-24 at 80-110 DEG C H, reaction terminates rear blowing, by clean for porogen extracting after drying, obtains product.
A kind of preparation purifying vanadium adsorbing material the most according to claim 1, it is characterised in that described porogen is white oil, molten Agent oil, one or more of toluene.
CN201610408025.4A 2016-06-13 2016-06-13 Preparation method of purified vanadium adsorption material Withdrawn CN105833854A (en)

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106188375A (en) * 2016-08-21 2016-12-07 王琪宇 A kind of preparation method of vitamin K3 purification adsorbent
CN106179275A (en) * 2016-08-21 2016-12-07 王金桢 A kind of preparation method of vinylene carbonate purification adsorbent
CN106215865A (en) * 2016-08-21 2016-12-14 王琪宇 A kind of preparation method of menatetrenone purification adsorbent
CN106215894A (en) * 2016-08-21 2016-12-14 王琪宇 A kind of preparation method of lysine purification adsorbent
CN106311150A (en) * 2016-08-21 2017-01-11 王金桢 Preparation method of adsorbent for purification of trimethylolpropane trioleate
CN106311169A (en) * 2016-08-21 2017-01-11 王金桢 Preparation method of adsorbent for purifying lincomycin hydrochloride
CN106349077A (en) * 2016-08-21 2017-01-25 王琪宇 Preparation method of adsorbent for purifying trimethylolpropane oleate
CN106902768A (en) * 2016-08-21 2017-06-30 王琪宇 A kind of trimesic acid purification aids
CN106916253A (en) * 2016-08-21 2017-07-04 王琪宇 A kind of dialkyl carbonate purification aids
CN106944015A (en) * 2016-08-21 2017-07-14 王琪宇 A kind of mizoribine purifies used additives
CN107011385A (en) * 2016-08-21 2017-08-04 王琪宇 A kind of hexachlorocyclotriph,sphazene purifies the preparation method of auxiliary agent
CN107022003A (en) * 2016-08-21 2017-08-08 王琪宇 A kind of preparation method of colistin sulfate scarvenger
CN107051409A (en) * 2016-08-21 2017-08-18 王琪宇 A kind of tannic acid purifies the preparation method of auxiliary agent
CN107051395A (en) * 2016-08-21 2017-08-18 王琪宇 A kind of gemcitabine hydrochloride purifies the preparation method of auxiliary agent
CN107138142A (en) * 2016-08-21 2017-09-08 王琪宇 A kind of preparation method of phenylstilbene bromide scarvenger
CN107138141A (en) * 2016-08-21 2017-09-08 王金桢 A kind of preparation method of purifying germane auxiliary agent
CN107159159A (en) * 2016-08-21 2017-09-15 王琪宇 A kind of preparation method of dodecanedioic acid used additives

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101062785A (en) * 2006-04-26 2007-10-31 中南大学 Method for deeply removing vanadium of vanadium-containing molybdate solution
CN102161757A (en) * 2011-03-08 2011-08-24 上海树脂厂有限公司 Special resin for vanadium extraction and preparation method thereof
CN102583822A (en) * 2012-02-09 2012-07-18 湖南大学 Method for removing heavy metal ion in waste water generated by vanadium extraction
CN103752288A (en) * 2014-01-22 2014-04-30 王金明 Preparation method of adsorbent applied to rapamycin separation
CN103772575A (en) * 2014-01-22 2014-05-07 王金明 Method for preparing parting material for extracting lithium
CN104744614A (en) * 2013-12-25 2015-07-01 浙江衢州万能达科技有限公司 Preparation method of resin for extracting vanadium from stone coal
CN105056905A (en) * 2015-07-08 2015-11-18 王金明 Preparation method of vanadium pentoxide adsorbent
CN105294910A (en) * 2015-11-30 2016-02-03 王金明 Preparation method of sorbent applied to pristinamycin separation
CN105294922A (en) * 2015-11-30 2016-02-03 王金明 Lithium separation material preparation method

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101062785A (en) * 2006-04-26 2007-10-31 中南大学 Method for deeply removing vanadium of vanadium-containing molybdate solution
CN102161757A (en) * 2011-03-08 2011-08-24 上海树脂厂有限公司 Special resin for vanadium extraction and preparation method thereof
CN102583822A (en) * 2012-02-09 2012-07-18 湖南大学 Method for removing heavy metal ion in waste water generated by vanadium extraction
CN104744614A (en) * 2013-12-25 2015-07-01 浙江衢州万能达科技有限公司 Preparation method of resin for extracting vanadium from stone coal
CN103752288A (en) * 2014-01-22 2014-04-30 王金明 Preparation method of adsorbent applied to rapamycin separation
CN103772575A (en) * 2014-01-22 2014-05-07 王金明 Method for preparing parting material for extracting lithium
CN105056905A (en) * 2015-07-08 2015-11-18 王金明 Preparation method of vanadium pentoxide adsorbent
CN105294910A (en) * 2015-11-30 2016-02-03 王金明 Preparation method of sorbent applied to pristinamycin separation
CN105294922A (en) * 2015-11-30 2016-02-03 王金明 Lithium separation material preparation method

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106188375A (en) * 2016-08-21 2016-12-07 王琪宇 A kind of preparation method of vitamin K3 purification adsorbent
CN106179275A (en) * 2016-08-21 2016-12-07 王金桢 A kind of preparation method of vinylene carbonate purification adsorbent
CN106215865A (en) * 2016-08-21 2016-12-14 王琪宇 A kind of preparation method of menatetrenone purification adsorbent
CN106215894A (en) * 2016-08-21 2016-12-14 王琪宇 A kind of preparation method of lysine purification adsorbent
CN106311150A (en) * 2016-08-21 2017-01-11 王金桢 Preparation method of adsorbent for purification of trimethylolpropane trioleate
CN106311169A (en) * 2016-08-21 2017-01-11 王金桢 Preparation method of adsorbent for purifying lincomycin hydrochloride
CN106349077A (en) * 2016-08-21 2017-01-25 王琪宇 Preparation method of adsorbent for purifying trimethylolpropane oleate
CN106902768A (en) * 2016-08-21 2017-06-30 王琪宇 A kind of trimesic acid purification aids
CN106916253A (en) * 2016-08-21 2017-07-04 王琪宇 A kind of dialkyl carbonate purification aids
CN106944015A (en) * 2016-08-21 2017-07-14 王琪宇 A kind of mizoribine purifies used additives
CN107011385A (en) * 2016-08-21 2017-08-04 王琪宇 A kind of hexachlorocyclotriph,sphazene purifies the preparation method of auxiliary agent
CN107022003A (en) * 2016-08-21 2017-08-08 王琪宇 A kind of preparation method of colistin sulfate scarvenger
CN107051409A (en) * 2016-08-21 2017-08-18 王琪宇 A kind of tannic acid purifies the preparation method of auxiliary agent
CN107051395A (en) * 2016-08-21 2017-08-18 王琪宇 A kind of gemcitabine hydrochloride purifies the preparation method of auxiliary agent
CN107138142A (en) * 2016-08-21 2017-09-08 王琪宇 A kind of preparation method of phenylstilbene bromide scarvenger
CN107138141A (en) * 2016-08-21 2017-09-08 王金桢 A kind of preparation method of purifying germane auxiliary agent
CN107159159A (en) * 2016-08-21 2017-09-15 王琪宇 A kind of preparation method of dodecanedioic acid used additives

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Application publication date: 20160810