CN107715851A - A kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron - Google Patents

A kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron Download PDF

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CN107715851A
CN107715851A CN201710820495.6A CN201710820495A CN107715851A CN 107715851 A CN107715851 A CN 107715851A CN 201710820495 A CN201710820495 A CN 201710820495A CN 107715851 A CN107715851 A CN 107715851A
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parts
weight
vingon
high adsorption
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CN107715851B (en
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王东
叶挺刚
蒋海托
余永刚
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Tongling yizhida technology achievement transformation Co., Ltd
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Tongling Hai Yuan Ultrafine Powder Co Ltd
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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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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 surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
    • B01J20/3285—Coating or impregnation layers comprising different type of functional groups or interactions, e.g. different ligands in various parts of the sorbent, mixed mode, dual zone, bimodal, multimodal, ionic or hydrophobic, cationic or anionic, hydrophilic or hydrophobic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or 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 halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or 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 halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04—Characterised by the use of homopolymers or 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 halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron, first iron oxide particles are acidified with hydrochloric acid, then dropwise addition tetraethyl orthosilicate after water carries out ball milling with the mixed liquor of ethanol and ammoniacal liquor is added to be reacted, then reaction condition is kept to be sintered after adding lauryl amine reaction, it is redispersed in the mixed solution of gelatin and ethanol and adds after Vingon powder dissolved, heating is reacted, after addition white oil carries out mixing hot pressing with toluene as pore-foaming agent, both obtained after pore-foaming agent processing is removed to product, product specific surface area and high mechanical strength prepared by the present invention, service life is grown, with microcellular structure, with good mechanical property, high adsorption and hydrophobicity.

Description

A kind of preparation of the composite microporous Vingon material of high adsorption modified oxidized iron Method
Technical field
The invention belongs to field of compound material, and in particular to a kind of high adsorption modified oxidized iron is composite microporous to gather inclined chloroethene The preparation method of alkene material.
Background technology
Polyvinylidene chloride resin is the high polymer material for having high obstructing performance, and its barrier property is common packaging materials Tens times even hundred times.It also has self-extinguishment, oil resistivity and protects taste, and protection against the tide, fungicidal properties are also very excellent, especially It is that it has low-temperature heat-sealing and heat-shrinkable, and is easy to print, therefore be one of plastics that modern packaging industry is favored, extensively For the packaging of food, medicine, precision instrument and various military articles for use, " green " packaging material is described as.In addition, with the resin Manufactured latex has preferable anti-flammability and cohesiveness, thus is also widely used on building materials and fireproof coating.
Carbon molecular sieve is a kind of novel carbon material that early seventies grow up, and it is as a kind of excellent absorption Agent, it is valued by the people, and has been supplied in the industries such as stone sleeve chemical environment improvement and thermomechanical aging, especially carbon point Son sieve more shows superiority in the nitrogen production by air separation of pressure swing adsorption technique.Carbon molecular sieve claims carbon black bead or carbon porous small ball, Its chemical composition is carbonization Vingon, is non-polar compound, is the carrier of gas-chromatography.Prepare the raw material of carbon molecular sieve A lot, source is also very wide.Different preparation technologies can be passed through by different original materials in theory, obtain pore radiuses and distribution Different carbon molecular sieve.Experiment shows that the raw material of low ash content, high carbon content and high volatile is relatively adapted to prepare high-performance Carbon molecular sieve.
Porous material turns into the fields such as catalysis, electrochemistry and absorption because of the duct with big specific surface area and insertion Focus material, the controllable preparation research of porous material attract the concern of many researchers.At present porous material is prepared to adopt Synthetic method mainly has template and template-free method.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided a kind of high adsorption modified oxidized iron is compound micro- The preparation method of hole Vingon material, product specific surface area and high mechanical strength, the service life length of preparation, has micropore Structure, there is good mechanical property, high adsorption and hydrophobicity.
The present invention is achieved by the following technical solutions：
A kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron, comprises the following steps：
（1）5-10 parts by weight iron oxide is added and soaked in appropriate hydrochloric acid solution 20-50 minutes, magnet adsorption takes out cleaning, 15-25 parts by weight water is added, the ammoniacal liquor of 50-60 parts by weight of ethanol and 1-5 parts by weight, ball milling mixing 5-8 hours, adds 0.1- 0.3 parts by weight tetraethyl orthosilicate, 4-8 hours are stirred at room temperature under nitrogen protection, it is stand-by；
（2）To step（1）Add 0.5-2 parts by weight lauryl amine in gained particle to add in above-mentioned solution, magnetic agitation mixing is equal It is even, after forming clear transparent solutions, sintered after carrying out ball milling 6-10 hours, it is stand-by；
（3）By step（2）Gains are dispersed in 5-10 parts by weight gelatin, in 40-60 parts by weight of ethanol, add 10-20 parts by weight Vingon powder be stirred dissolving, then heat to 75-85 DEG C reaction 12-16 hours, at room temperature stand 18-24 it is small When, it is stand-by；
（4）By step（3）Gains add 2-5 parts by weight white oils, 2-8 parts by weight methyl isobutyl carbinols, at 70 DEG C -100 DEG C After reacting 12-24 hours, two-roll mill be kneaded 5-15 minutes and prolongs and be pressed into after flaky composite material through vulcanizing press heat After pressing 5-20 minutes, extraction toluene, white oil, drying closing bag both obtain the composite microporous Vingon material of high adsorption modified oxidized iron Material.
Described step（2）In be sintered to 800 DEG C be warming up to from 25 DEG C, heating rate is 1-2.5 DEG C/min, is incubated 2- 4 hours, sintered in air, then cool to normal temperature with the furnace.
Described step（4）It is that temperature is 160-180 DEG C that two-roll mill, which carries out compounding conditions, front and rear roller slewing rate ratio For 1:(1-1.2).
Described step（4）Vulcanizing press hot pressing condition is that temperature is 180-200 DEG C, pressure 10-20MPa.
Described step（4）Extract toluene, white oil is product to be added in 80-100 parts by weight solvent oil, in 60-70 DEG C reaction 2-4 hours.
It is an advantage of the invention that：
Iron oxide particles are first acidified by the present invention with hydrochloric acid, are then added water and are carried out ball milling with the mixed liquor of ethanol and ammoniacal liquor Tetraethyl orthosilicate is added dropwise afterwards to be reacted, then keeps reaction condition to be sintered after adding lauryl amine reaction, is redispersed in After addition Vingon powder is dissolved in the mixed solution of gelatin and ethanol, heating is reacted, and adds white oil and first After benzene carries out mixing hot pressing as pore-foaming agent, both obtained after pore-foaming agent processing is removed to product, the iron oxide being acidified after ball milling For particle in the presence of ammoniacal liquor, tetraethyl orthosilicate is coated on iron oxide particles surface by sol-gel process, forms dioxy SiClx layer, the lauryl amine of addition form the porous oxidation of Surface coating silicon dioxide layer as sintering after precipitating reagent deposition of iron oxide Iron, hydrophobic effect and adsorptivity are improved, after adding Vingon progress copolymerized grafting, modified oxidized iron particle is poly- inclined Good in vinyl chloride to disperse, adding pore-foaming agent makes material form carbon molecular sieve micropore structure, can be with stable metal ion with carrying High adsorption, the product specific surface area for preparing of the present invention and high mechanical strength, service life length, have microcellular structure, with good Good mechanical property, high adsorption and hydrophobicity.
Embodiment
A kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron, comprises the following steps：
（1）8 parts by weight iron oxide are added in appropriate hydrochloric acid solution and soaked 35 minutes, magnet adsorption takes out cleaning, adds 20 Parts by weight water, the ammoniacal liquor of 55 parts by weight of ethanol and 2 parts by weight, ball milling mixing 6 hours, 0.2 parts by weight tetraethyl orthosilicate is added, It is stirred at room temperature 6 hours under nitrogen protection, it is stand-by；
（2）To step（1）1.2 parts by weight lauryl amines are added in gained particle to add in above-mentioned solution, magnetic agitation is well mixed, After forming clear transparent solutions, ball milling is carried out after 8 hours, is sintered, it is stand-by；
（3）By step（2）Gains are dispersed in 8 parts by weight gelatin, in 50 parts by weight of ethanol, add the poly- inclined chloroethene of 15 parts by weight Alkene powder is stirred dissolving, then heats to 80 DEG C and reacts 14 hours, stands 20 hours at room temperature, stand-by；
（4）By step（3）Gains add 3 parts by weight white oils, 5 parts by weight methyl isobutyl carbinols, are reacted 18 hours at 85 DEG C Afterwards, two-roll mill be kneaded prolonging for 10 minutes and is pressed into after flaky composite material after vulcanizing press hot pressing 15 minutes, is extracted Toluene, white oil, drying closing bag both obtain the composite microporous Vingon material of high adsorption modified oxidized iron.
Described step（2）In be sintered to 800 DEG C be warming up to from 25 DEG C, heating rate is 1.5 DEG C/min, and insulation 3 is small When, sinter in air, then cool to normal temperature with the furnace.
Described step（4）It is that temperature is 170 DEG C that two-roll mill, which carries out compounding conditions, and front and rear roller slewing rate ratio is 1: 1.1。
Described step（4）Vulcanizing press hot pressing condition is that temperature is 190 DEG C, pressure 15MPa.
Described step（4）Extraction toluene, white oil are that product is added in 90 parts by weight solvent oil, react 3 in 65 DEG C Hour.

Claims (5)

  1. A kind of 1. preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron, it is characterised in that including Following steps：
    （1）5-10 parts by weight iron oxide is added and soaked in appropriate hydrochloric acid solution 20-50 minutes, magnet adsorption takes out cleaning, 15-25 parts by weight water is added, the ammoniacal liquor of 50-60 parts by weight of ethanol and 1-5 parts by weight, ball milling mixing 5-8 hours, adds 0.1- 0.3 parts by weight tetraethyl orthosilicate, 4-8 hours are stirred at room temperature under nitrogen protection, it is stand-by；
    （2）To step（1）Add 0.5-2 parts by weight lauryl amine in gained particle to add in above-mentioned solution, magnetic agitation mixing is equal It is even, after forming clear transparent solutions, sintered after carrying out ball milling 6-10 hours, it is stand-by；
    （3）By step（2）Gains are dispersed in 5-10 parts by weight gelatin, in 40-60 parts by weight of ethanol, add 10-20 parts by weight Vingon powder be stirred dissolving, then heat to 75-85 DEG C reaction 12-16 hours, at room temperature stand 18-24 it is small When, it is stand-by；
    （4）By step（3）Gains add 2-5 parts by weight white oils, 2-8 parts by weight methyl isobutyl carbinols, at 70 DEG C -100 DEG C After reacting 12-24 hours, two-roll mill be kneaded 5-15 minutes and prolongs and be pressed into after flaky composite material through vulcanizing press heat After pressing 5-20 minutes, extraction toluene, white oil, drying closing bag both obtain the composite microporous Vingon material of high adsorption modified oxidized iron Material.
  2. 2. according to a kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron of claim 1, its It is characterised by, described step（2）In be sintered to 800 DEG C be warming up to from 25 DEG C, heating rate is 1-2.5 DEG C/min, insulation 2-4 hours, sinter in air, then cool to normal temperature with the furnace.
  3. 3. according to a kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron of claim 1, its It is characterised by, described step（4）It is that temperature is 160-180 DEG C that two-roll mill, which carries out compounding conditions, front and rear roller slewing rate Than for 1:(1-1.2).
  4. 4. according to a kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron of claim 1, its It is characterised by, described step（4）Vulcanizing press hot pressing condition is that temperature is 180-200 DEG C, pressure 10-20MPa.
  5. 5. according to a kind of preparation method of the composite microporous Vingon material of high adsorption modified oxidized iron of claim 1, its It is characterised by, described step（4）Extract toluene, white oil is product to be added in 80-100 parts by weight solvent oil, in 60- 70 DEG C of reaction 2-4 hours.
CN201710820495.6A 2017-09-13 2017-09-13 Preparation method of high-adsorptivity modified iron oxide composite microporous polyvinylidene chloride material Active CN107715851B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186762A (en) * 2007-12-03 2008-05-28 南京大学 Method for enwrapping ferric oxide by silicon dioxide
CN101306327A (en) * 2008-07-08 2008-11-19 大连理工大学 Spiral carbon membrane and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186762A (en) * 2007-12-03 2008-05-28 南京大学 Method for enwrapping ferric oxide by silicon dioxide
CN101306327A (en) * 2008-07-08 2008-11-19 大连理工大学 Spiral carbon membrane and preparation method thereof

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