CN106905651B - The modified PVPP/TiO of cromoci Selective Separation in animal viscera2Nanocomposite - Google Patents

The modified PVPP/TiO of cromoci Selective Separation in animal viscera2Nanocomposite Download PDF

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CN106905651B
CN106905651B CN201710216766.7A CN201710216766A CN106905651B CN 106905651 B CN106905651 B CN 106905651B CN 201710216766 A CN201710216766 A CN 201710216766A CN 106905651 B CN106905651 B CN 106905651B
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pvpp
tio
modified
cromoci
nano
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CN106905651A (en
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孙凯
王静
闫磊
王妍
桂金秋
蔡克瑞
刘春玲
齐悦
宋洁
晁岳刚
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Mudanjiang Medical University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L39/00—Compositions 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 single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions of derivatives of such polymers
    • C08L39/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
    • C08L39/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
    • B01D15/424—Elution mode
    • B01D15/426—Specific type of solvent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a kind of modified PVPP/TiO of cromoci Selective Separation in animal viscera2Nanocomposite, is related to biomedicine technical field, and specific preparation method includes the following steps: (1) nano-TiO2Powder pretreatment, the preparation of (2) modified PVPP, (3) modified PVPP/TiO2The preparation of nanocomposite.The made modified PVPP/TiO of the present invention2Nanocomposite is exclusively used in the Selective Separation of cromoci in animal viscera, selectively reaches 85%, and adsorption efficiency is up to 89%, adsorbed cromoci is through Na3PO4Treated that elution efficiency reaches 95% for eluant, eluent, to realize that animal viscera acid mentions efficiently separating for cromoci in solution, greatly improves the yield of cromoci.

Description

The modified PVPP/TiO of cromoci Selective Separation in animal viscera2It is nano combined Material
Technical field:
The present invention relates to biomedicine technical fields, and in particular to cromoci Selective Separation in a kind of animal viscera With modified PVPP/TiO2Nanocomposite.
Background technique:
Cromoci is the electron transit mediator in biological oxidation process.Its action principle be in the presence of enzyme, Oxidation, also original rapid rush enzyme effect to tissue.Usual exogenous cytochrome C not can enter healthy cell, but lack Permeability of cell membranes increases when oxygen, and cromoci is just likely to enter in cell and mitochondria, enhances cellular oxidation, can mention The utilization of hyperoxia.Studies have shown that cromoci can be used in first aid and the adjuvant drug of histanoxia, as anthracemia, Expiratory dyspnea caused by hypnotics poisoning, asphyxia neonatorum, serious shock anoxic, anesthesia and pulmonary disease, mountain hypoxia, brain lack Anoxic caused by oxygen, heart disease etc..
Isolate and purify from animal viscera is to prepare one of approach of cromoci.Since cromoci is a kind of stabilization Soluble protein, soluble easily in water, solubility is bigger in an acidic solution, therefore common acid solution extracts.Utilize adsorptivity object Matter proposes one of the mode that selective absorption cromoci in solution is quick separating cromoci from acid, has adsorbed cytochromes The adsorbability material of C is eluted through eluant, eluent again, obtains the eluant, eluent containing cromoci.Currently, having been reported that using artificial Zeolite is as adsorbability material, but that there are the adsorption efficiencies of institute adherent cell pigment C is low, elution efficiency is low after eluent The problem of, it is difficult to the cromoci of high-content is obtained, therefore needs to develop the high adsorptivity of adsorption efficiency and elution efficiency Substance.
Summary of the invention:
Technical problem to be solved by the present invention lies in provide a kind of adsorption efficiency and that elution efficiency is high, selectivity is strong is dynamic The modified PVPP/TiO of cromoci Selective Separation in object internal organs2Nanocomposite.
The following technical solution is employed for the technical problems to be solved by the invention to realize:
The modified PVPP/TiO of cromoci Selective Separation in animal viscera2Nanocomposite, specific preparation method Include the following steps:
(1) nano-TiO2Powder pretreatment: to nano-TiO2Aromatic modified terpene resin and double fluoroforms are added in powder Sulfimide is warming up to 70-80 DEG C of heat preservation mixing 5-10min after being sufficiently mixed with the heating rate of 5 DEG C/min, then with 5 DEG C/ The cooling rate of min is cooled to 0-5 DEG C of heat preservation and stands 1-2h, is then warming up to 100-110 DEG C with the heating rate of 10 DEG C/min Heat preservation mixing 10-15min is finally warming up to 500-550 DEG C of heat preservation roasting 2-3h；
(2) microcrystalline cellulose cross-linked polyacrylamide the preparation of modified PVPP: is added into crosslinked polyvinylpyrrolidone And polyvinyl butyral, microwave treater microwave treatment 5-10min is utilized after being sufficiently mixed, and adds hexamethylol melamine Amine pregnancy ether continues microwave treatment 3-5min, gained mixture is transferred in 0-5 DEG C of environment rapidly after microwave treatment and is sealed 0.5-1h is stood, 50-60 DEG C of warm water is then added under stiring, and reflux state is warming up to the heating rate of 5 DEG C/min and is protected Gained mixed solution, is sent into spray dryer by temperature stirring 10-15min after naturally cool to after room temperature, dry gained particle Micro mist is made to get modified PVPP through micronizer；
(3) modified PVPP/TiO2The preparation of nanocomposite: to nano-TiO after pretreatment2Institute is added in powder Modified PVPP is made, microwave treater microwave treatment 5-10min is utilized after being sufficiently mixed, and stand 0.5- in 15-20 DEG C of environment 1h, microwave treatment 3-5min, is then added polyethylene glycol oxide and ferrocene again, continues microwave treatment 5- after mixing Gained mixture is sent into high energy ball mill by 10min after naturally cool to after 45-50 DEG C, ground to be made powdered and change Property PVPP/TiO2Nanocomposite.
Nano-TiO in the step (1)2The weight of powder, aromatic modified terpene resin and double trifluoromethanesulfonimides Amount ratio is 15-20:0.5-1:0.1-0.2.
Aromatic modified terpene resin is formed by terpene resin through anthracene modification in the step (1), it is specific the preparation method comprises the following steps: Anthracene is dissolved in ethyl alcohol, terpene resin, hydrogenated palm oil and titanate coupling agent are added, stirring is quiet after so that it is uniformly dispersed 10-15min is set, and reflux state heat preservation mixing 0.5-1h is warming up to the heating rate of 5 DEG C/min, after naturally cool to 40- It is sent into spray dryer after 45 DEG C, hydrolysis of polymaleic anhydride then is added into dry gained particle, again with 5 DEG C/min's Heating rate is warming up to 120-125 DEG C of heat preservation mixing 0.5-1h, and last cooled to room temperature is to get aromatic modified terpenes tree Rouge.
The anthracene, ethyl alcohol, terpene resin, hydrogenated palm oil, the weight use of titanate coupling agent and hydrolysis of polymaleic anhydride Amount is than being 5-10:50-80:15-20:0.5-1:0.05-0.1:0.5-1.
Crosslinked polyvinylpyrrolidone, microcrystalline cellulose cross-linked polyacrylamide, polyvinyl alcohol contracting fourth in the step (2) The weight consumption ratio of aldehyde, hexamethylolmelamine pregnancy ether and water is 10-15:1-2:0.5-1:0.3-0.5:30-50.
Microcrystalline cellulose cross-linked polyacrylamide is passed through by microcrystalline cellulose and cationic polyacrylamide in the step (2) Physical crosslinking is made, specific the preparation method comprises the following steps: cationic polyacrylamide and poloxamer are dissolved in the water, and with 5 DEG C/ The heating rate of min is warming up to reflux state insulated and stirred 5-10min, adds microcrystalline cellulose and nanometer rubber powder, continues back Insulated and stirred 0.5-1h is flowed, is then cooled to 35-45 DEG C with the cooling rate of 10 DEG C/min, gained mixed liquor is sent into freeze-drying In machine, micro mist is made through micronizer to get microcrystalline cellulose cross-linked polyacrylamide in dry obtained solid.
The cationic polyacrylamide, poloxamer, water, microcrystalline cellulose and nanometer rubber powder weight consumption ratio be 5- 10:0.5-1:15-30:3-5:0.1-0.3。
Nano-TiO in the step (3)2Powder, the weight consumption ratio for being modified PVPP, polyethylene glycol oxide and ferrocene are 25-30:5-10:0.5-1:0.05-0.1。
The operating condition of the microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
The beneficial effects of the present invention are: the made modified PVPP/TiO of the present invention2Nanocomposite is exclusively used in animal viscera The Selective Separation of middle cromoci, animal viscera acid can be carried out by, which being filled with being made after adsorption column, mentions cell color in solution The selective absorption of plain C selectively reaches 85%, and adsorption efficiency is up to 89%, and adsorbed cromoci is through Na3PO4 Treated that elution efficiency reaches 98% for eluant, eluent, thus realize that animal viscera acid mentions efficiently separating for cromoci in solution, Greatly improve the yield of cromoci.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) nano-TiO2Powder pretreatment: to 30 parts of nano-TiOs21 part of aromatic modified terpene resin and 0.3 is added in powder The double trifluoromethanesulfonimides of part are warming up to 70-80 DEG C of heat preservation mixing after being sufficiently mixed with the heating rate of 5 DEG C/min 10min, then 0-5 DEG C of heat preservation is cooled to the cooling rate of 5 DEG C/min and stands 1h, then heated up with the heating rate of 10 DEG C/min 15min is mixed to 100-110 DEG C of heat preservation, is finally warming up to 500-550 DEG C of heat preservation roasting 3h；
(2) 1 part of microcrystalline cellulose crosslinked polypropylene the preparation of modified PVPP: is added into 15 parts of crosslinked polyvinylpyrrolidone Acrylamide and 0.5 part of polyvinyl butyral utilize microwave treater microwave treatment 5min, add 0.3 part after being sufficiently mixed Hexamethylolmelamine pregnancy ether continues microwave treatment 5min, gained mixture is transferred to 0-5 rapidly after microwave treatment Then 50 parts of 50-60 DEG C of warm water are added in sealing and standing 1h in DEG C environment under stiring, and with the heating of the heating rate of 5 DEG C/min To reflux state insulated and stirred 15min, gained mixed solution is sent into spray dryer after naturally cool to after room temperature, it is dry Micro mist is made through micronizer to get modified PVPP in gained particle；
(3) modified PVPP/TiO2The preparation of nanocomposite: to 25 parts of nano-TiOs after pretreatment2Add in powder Enter 5 parts of made modified PVPP, microwave treater microwave treatment 5min is utilized after being sufficiently mixed, and stand in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is then added 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, continues after mixing micro- again Wave handles 5min, and gained mixture is sent into high energy ball mill after naturally cool to after 45-50 DEG C, ground to be made powdered Modification PVPP/TiO2Nanocomposite.
The preparation of aromatic modified terpene resin: 5 parts of anthracenes are dissolved in 80 parts of ethyl alcohol, add 15 parts of terpene resins, 0.5 Part hydrogenated palm oil and 0.05 part of titanate coupling agent, stirring stand 15 min after so that it is uniformly dispersed, and with the liter of 5 DEG C/min Warm speed be warming up to reflux state heat preservation mixing 1h, after naturally cool to after 40-45 DEG C be sent into spray dryer in, then to 0.5 part of hydrolysis of polymaleic anhydride is added in dry gained particle, is warming up to 120-125 DEG C again with the heating rate of 5 DEG C/min Heat preservation mixing 0.5h, last cooled to room temperature is to get aromatic modified terpene resin.
The preparation of microcrystalline cellulose cross-linked polyacrylamide: by 10 parts of cationic polyacrylamide and 0.5 part of poloxamer Be dissolved in 30 parts of water, and 10 min of reflux state insulated and stirred be warming up to the heating rate of 5 DEG C/min, add 5 parts it is micro- Crystalline cellulose and 0.1 part of nanometer rubber powder are continued the insulated and stirred 0.5h that flows back, are then cooled to the cooling rate of 10 DEG C/min 35-45 DEG C, gained mixed liquor is sent into freeze drier, and micro mist is made through micronizer to get crystallite in dry obtained solid Cellulose crosslinked polyacrylamide.
Wherein, the operating condition of microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
Embodiment 2
(1) nano-TiO2Powder pretreatment: to 35 parts of nano-TiOs21 part of aromatic modified terpene resin and 0.3 is added in powder The double trifluoromethanesulfonimides of part are warming up to 70-80 DEG C of heat preservation mixing after being sufficiently mixed with the heating rate of 5 DEG C/min 10min, then 0-5 DEG C of heat preservation is cooled to the cooling rate of 5 DEG C/min and stands 1h, then heated up with the heating rate of 10 DEG C/min 15min is mixed to 100-110 DEG C of heat preservation, is finally warming up to 500-550 DEG C of heat preservation roasting 3h；
(2) 2 parts of microcrystalline cellulose crosslinked polypropylenes the preparation of modified PVPP: are added into 15 parts of crosslinked polyvinylpyrrolidone Acrylamide and 0.5 part of polyvinyl butyral utilize microwave treater microwave treatment 5min, add 0.3 part after being sufficiently mixed Hexamethylolmelamine pregnancy ether continues microwave treatment 5min, gained mixture is transferred to 0-5 rapidly after microwave treatment Then 50 parts of 50-60 DEG C of warm water are added in sealing and standing 1h in DEG C environment under stiring, and with the heating of the heating rate of 5 DEG C/min To reflux state insulated and stirred 15min, gained mixed solution is sent into spray dryer after naturally cool to after room temperature, it is dry Micro mist is made through micronizer to get modified PVPP in gained particle；
(3) modified PVPP/TiO2The preparation of nanocomposite: to 30 parts of nano-TiOs after pretreatment2Add in powder Enter 5 parts of made modified PVPP, microwave treater microwave treatment 5min is utilized after being sufficiently mixed, and stand in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is then added 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, continues after mixing micro- again Wave handles 5min, and gained mixture is sent into high energy ball mill after naturally cool to after 45-50 DEG C, ground to be made powdered Modification PVPP/TiO2Nanocomposite.
The preparation of aromatic modified terpene resin: 5 parts of anthracenes are dissolved in 80 parts of ethyl alcohol, add 20 parts of terpene resins, 0.5 Part hydrogenated palm oil and 0.05 part of titanate coupling agent, stirring stand 15 min after so that it is uniformly dispersed, and with the liter of 5 DEG C/min Warm speed be warming up to reflux state heat preservation mixing 1h, after naturally cool to after 40-45 DEG C be sent into spray dryer in, then to 1 part of hydrolysis of polymaleic anhydride is added in dry gained particle, 120-125 DEG C of guarantor is warming up to the heating rate of 5 DEG C/min again Temperature mixing 0.5h, last cooled to room temperature is to get aromatic modified terpene resin.
The preparation of microcrystalline cellulose cross-linked polyacrylamide: by 10 parts of cationic polyacrylamide and 0.5 part of poloxamer Be dissolved in 30 parts of water, and 10 min of reflux state insulated and stirred be warming up to the heating rate of 5 DEG C/min, add 3 parts it is micro- Crystalline cellulose and 0.2 part of nanometer rubber powder are continued the insulated and stirred 0.5h that flows back, are then cooled to the cooling rate of 10 DEG C/min 35-45 DEG C, gained mixed liquor is sent into freeze drier, and micro mist is made through micronizer to get crystallite in dry obtained solid Cellulose crosslinked polyacrylamide.
Wherein, the operating condition of microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
Reference examples 1
(1) nano-TiO2Powder pretreatment: to 35 parts of nano-TiOs21 part of aromatic modified terpene resin and 0.3 is added in powder The double trifluoromethanesulfonimides of part are warming up to 70-80 DEG C of heat preservation mixing after being sufficiently mixed with the heating rate of 5 DEG C/min 10min, then 0-5 DEG C of heat preservation is cooled to the cooling rate of 5 DEG C/min and stands 1h, then heated up with the heating rate of 10 DEG C/min 15min is mixed to 100-110 DEG C of heat preservation, is finally warming up to 500-550 DEG C of heat preservation roasting 3h；
(2) preparation of modified PVPP: be added into 15 parts of crosslinked polyvinylpyrrolidone 2 parts of cationic polyacrylamide and 0.5 part of polyvinyl butyral utilizes microwave treater microwave treatment 5min, adds 0.3 part of hexamethylol after being sufficiently mixed Melamine pregnancy ether continues microwave treatment 5min, gained mixture is transferred in 0-5 DEG C of environment rapidly after microwave treatment Then 50 parts of 50-60 DEG C of warm water are added under stiring, and are warming up to reflux shape with the heating rate of 5 DEG C/min by sealing and standing 1h Gained mixed solution is sent into spray dryer by state insulated and stirred 15min after naturally cool to after room temperature, dry gained particle Micro mist is made to get modified PVPP through micronizer；
(3) modified PVPP/TiO2The preparation of nanocomposite: to 30 parts of nano-TiOs after pretreatment2Add in powder Enter 5 parts of made modified PVPP, microwave treater microwave treatment 5min is utilized after being sufficiently mixed, and stand in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is then added 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, continues after mixing micro- again Wave handles 5min, and gained mixture is sent into high energy ball mill after naturally cool to after 45-50 DEG C, ground to be made powdered Modification PVPP/TiO2Nanocomposite.
The preparation of aromatic modified terpene resin: 5 parts of anthracenes are dissolved in 80 parts of ethyl alcohol, add 20 parts of terpene resins, 0.5 Part hydrogenated palm oil and 0.05 part of titanate coupling agent, stirring stand 15 min after so that it is uniformly dispersed, and with the liter of 5 DEG C/min Warm speed be warming up to reflux state heat preservation mixing 1h, after naturally cool to after 40-45 DEG C be sent into spray dryer in, then to 1 part of hydrolysis of polymaleic anhydride is added in dry gained particle, 120-125 DEG C of guarantor is warming up to the heating rate of 5 DEG C/min again Temperature mixing 0.5h, last cooled to room temperature is to get aromatic modified terpene resin.
Wherein, the operating condition of microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
Reference examples 2
(1) nano-TiO2Powder pretreatment: to 35 parts of nano-TiOs21 part of terpene resin and 0.3 part double three are added in powder Fluoromethane sulfimide is warming up to 70-80 DEG C of heat preservation mixing 10min after being sufficiently mixed with the heating rate of 5 DEG C/min, then with 5 DEG C/cooling rate of min is cooled to 0-5 DEG C of heat preservation and stands 1h, 100-110 is then warming up to the heating rate of 10 DEG C/min DEG C heat preservation mixing 15min, is finally warming up to 500-550 DEG C of heat preservation and roasts 3h；
(2) 2 parts of microcrystalline cellulose crosslinked polypropylenes the preparation of modified PVPP: are added into 15 parts of crosslinked polyvinylpyrrolidone Acrylamide and 0.5 part of polyvinyl butyral utilize microwave treater microwave treatment 5min, add 0.3 part after being sufficiently mixed Hexamethylolmelamine pregnancy ether continues microwave treatment 5min, gained mixture is transferred to 0-5 rapidly after microwave treatment Then 50 parts of 50-60 DEG C of warm water are added in sealing and standing 1h in DEG C environment under stiring, and with the heating of the heating rate of 5 DEG C/min To reflux state insulated and stirred 15min, gained mixed solution is sent into spray dryer after naturally cool to after room temperature, it is dry Micro mist is made through micronizer to get modified PVPP in gained particle；
(3) modified PVPP/TiO2The preparation of nanocomposite: to 30 parts of nano-TiOs after pretreatment2Add in powder Enter 5 parts of made modified PVPP, microwave treater microwave treatment 5min is utilized after being sufficiently mixed, and stand in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is then added 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, continues after mixing micro- again Wave handles 5min, and gained mixture is sent into high energy ball mill after naturally cool to after 45-50 DEG C, ground to be made powdered Modification PVPP/TiO2Nanocomposite.
The preparation of microcrystalline cellulose cross-linked polyacrylamide: by 10 parts of cationic polyacrylamide and 0.5 part of poloxamer Be dissolved in 30 parts of water, and 10 min of reflux state insulated and stirred be warming up to the heating rate of 5 DEG C/min, add 3 parts it is micro- Crystalline cellulose and 0.2 part of nanometer rubber powder are continued the insulated and stirred 0.5h that flows back, are then cooled to the cooling rate of 10 DEG C/min 35-45 DEG C, gained mixed liquor is sent into freeze drier, and micro mist is made through micronizer to get crystallite in dry obtained solid Cellulose crosslinked polyacrylamide.
Wherein, the operating condition of microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
Reference examples 3
(1) 2 parts of microcrystalline cellulose crosslinked polypropylenes the preparation of modified PVPP: are added into 15 parts of crosslinked polyvinylpyrrolidone Acrylamide and 0.5 part of polyvinyl butyral utilize microwave treater microwave treatment 5min, add 0.3 part after being sufficiently mixed Hexamethylolmelamine pregnancy ether continues microwave treatment 5min, gained mixture is transferred to 0-5 rapidly after microwave treatment Then 50 parts of 50-60 DEG C of warm water are added in sealing and standing 1h in DEG C environment under stiring, and with the heating of the heating rate of 5 DEG C/min To reflux state insulated and stirred 15min, gained mixed solution is sent into spray dryer after naturally cool to after room temperature, it is dry Micro mist is made through micronizer to get modified PVPP in gained particle；
(2) modified PVPP/TiO2The preparation of nanocomposite: to 30 parts of nano-TiOs25 parts of made modifications are added in powder PVPP utilizes microwave treater microwave treatment 5min, and stands 0.5h in 15-20 DEG C of environment after being sufficiently mixed, again microwave 5min is handled, 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene is then added, continues microwave treatment 5min after mixing, to Gained mixture is sent into high energy ball mill after naturally cooling to 45-50 DEG C, it is ground that powdered modification PVPP/ is made TiO2Nanocomposite.
The preparation of microcrystalline cellulose cross-linked polyacrylamide: by 10 parts of cationic polyacrylamide and 0.5 part of poloxamer Be dissolved in 30 parts of water, and 10 min of reflux state insulated and stirred be warming up to the heating rate of 5 DEG C/min, add 3 parts it is micro- Crystalline cellulose and 0.2 part of nanometer rubber powder are continued the insulated and stirred 0.5h that flows back, are then cooled to the cooling rate of 10 DEG C/min 35-45 DEG C, gained mixed liquor is sent into freeze drier, and micro mist is made through micronizer to get crystallite in dry obtained solid Cellulose crosslinked polyacrylamide.
Wherein, the operating condition of microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
Reference examples 4
Modified PVPP/TiO2The preparation of nanocomposite: to 30 parts of nano-TiOs25 parts of crosslinked polyethylenes are added in powder Pyrrolidones utilizes microwave treater microwave treatment 5min, and stands 0.5h in 15-20 DEG C of environment after being sufficiently mixed, again Then microwave treatment 5min is added 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, continues microwave treatment after mixing Gained mixture is sent into high energy ball mill by 5min after naturally cool to after 45-50 DEG C, ground that powdered modification is made PVPP/TiO2Nanocomposite.
Wherein, the operating condition of microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output power 700W。
Embodiment 3
It is utilized respectively equivalent embodiment 1, embodiment 2, reference examples 1, reference examples 2, reference examples 3 and the made modification of reference examples 4 PVPP/TiO2Nanocomposite mentions solution to same batch of equivalent Pigs Hearts acid and carries out the Selective Separation of cromoci, and is arranged Use equivalent nano-TiO2Powder is directly separated cromoci as reference examples 5, then uses 0.1mol/LNa3PO4Eluant, eluent pair The cromoci of absorption is eluted, while being measured to Selective Separation effect, and the results are shown in Table 1.
1 Pigs Hearts acid of table proposes the Selective Separation effect of cromoci in solution
Project Specific grain surface accumulates (m2/g) Selectivity (%) Adsorption efficiency (%) Elution efficiency (%)
Embodiment 1 199.27 85.34 89.26 98.15
Embodiment 2 197.85 83.12 87.31 98.22
Reference examples 1 158.66 70.41 68.12 87.34
Reference examples 2 143.74 52.06 55.50 80.53
Reference examples 3 124.58 41.23 49.34 72.26
Reference examples 4 102.43 30.52 38.27 64.40
Reference examples 5 85.12 18.33 21.65 56.61
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (7)

1. the modified PVPP/TiO of cromoci Selective Separation in animal viscera2Nanocomposite, which is characterized in that specific Preparation method includes the following steps:
(1) nano-TiO2Powder pretreatment: to nano-TiO2Aromatic modified terpene resin and double fluoroform sulphonyl are added in powder Imines is warming up to 70-80 DEG C of heat preservation mixing 5-10min after being sufficiently mixed with the heating rate of 5 DEG C/min, then with 5 DEG C/min's Cooling rate is cooled to 0-5 DEG C of heat preservation and stands 1-2h, and it is mixed to be then warming up to 100-110 DEG C of heat preservation with the heating rate of 10 DEG C/min 10-15min is closed, 500-550 DEG C of heat preservation roasting 2-3h is finally warming up to；
(2) preparation of modified PVPP: microcrystalline cellulose cross-linked polyacrylamide is added into crosslinked polyvinylpyrrolidone and gathers Vinyl butyral utilizes microwave treater microwave treatment 5-10min, adds hexamethylolmelamine six after being sufficiently mixed Methyl ether continues microwave treatment 3-5min, gained mixture is transferred to sealing and standing in 0-5 DEG C of environment rapidly after microwave treatment Then 50-60 DEG C of warm water is added under stiring, and is warming up to reflux state heat preservation with the heating rate of 5 DEG C/min and stirs by 0.5-1h 10-15min is mixed, gained mixed solution is sent into spray dryer after naturally cool to after room temperature, dry gained particle is through super Micro mist is made to get modified PVPP in atomizer；
(3) modified PVPP/TiO2The preparation of nanocomposite: to nano-TiO after pretreatment2Made change is added in powder Property PVPP, microwave treater microwave treatment 5-10min is utilized after being sufficiently mixed, and stands 0.5-1h in 15-20 DEG C of environment, then Then polyethylene glycol oxide and ferrocene is added in secondary microwave treatment 3-5min, continue microwave treatment 5-10min after mixing, to Gained mixture is sent into high energy ball mill after naturally cooling to 45-50 DEG C, it is ground that powdered modification PVPP/ is made TiO2Nanocomposite；
Aromatic modified terpene resin is formed by terpene resin through anthracene modification in the step (1), specifically the preparation method comprises the following steps: by anthracene It is dissolved in ethyl alcohol, adds terpene resin, hydrogenated palm oil and titanate coupling agent, stirring is stood after so that it is uniformly dispersed 10-15min, and reflux state heat preservation mixing 0.5-1h is warming up to the heating rate of 5 DEG C/min, after naturally cool to 40-45 It is sent into spray dryer after DEG C, hydrolysis of polymaleic anhydride then is added into dry gained particle, again with the liter of 5 DEG C/min Warm speed is warming up to 120-125 DEG C of heat preservation mixing 0.5-1h, and last cooled to room temperature is to get aromatic modified terpene resin；
Microcrystalline cellulose cross-linked polyacrylamide is by microcrystalline cellulose and cationic polyacrylamide through physics in the step (2) Crosslinking is made, specifically the preparation method comprises the following steps: cationic polyacrylamide and poloxamer are dissolved in the water, and with 5 DEG C/min Heating rate be warming up to reflux state insulated and stirred 5-10min, add microcrystalline cellulose and nanometer rubber powder, continue reflux protect Temperature stirring 0.5-1h, is then cooled to 35-45 DEG C with the cooling rate of 10 DEG C/min, gained mixed liquor is sent into freeze drier In, micro mist is made through micronizer to get microcrystalline cellulose cross-linked polyacrylamide in dry obtained solid.
2. the modified PVPP/TiO of cromoci Selective Separation in animal viscera according to claim 12It is nano combined Material, it is characterised in that: nano-TiO in the step (1)2Powder, aromatic modified terpene resin and double fluoroform sulphonyl are sub- The weight consumption ratio of amine is 15-20:0.5-1:0.1-0.2.
3. the modified PVPP/TiO of cromoci Selective Separation in animal viscera according to claim 12It is nano combined Material, it is characterised in that: the anthracene, ethyl alcohol, terpene resin, hydrogenated palm oil, titanate coupling agent and hydrolysis of polymaleic anhydride Weight consumption ratio be 5-10:50-80:15-20:0.5-1:0.05-0.1:0.5-1.
4. the modified PVPP/TiO of cromoci Selective Separation in animal viscera according to claim 12It is nano combined Material, it is characterised in that: crosslinked polyvinylpyrrolidone, microcrystalline cellulose cross-linked polyacrylamide, poly- second in the step (2) The weight consumption ratio of enol butyral, hexamethylolmelamine pregnancy ether and water is 10-15:1-2:0.5-1:0.3-0.5: 30-50。
5. the modified PVPP/TiO of cromoci Selective Separation in animal viscera according to claim 12It is nano combined Material, it is characterised in that: the weight use of the cationic polyacrylamide, poloxamer, water, microcrystalline cellulose and nanometer rubber powder Amount is than being 5-10:0.5-1:15-30:3-5:0.1-0.3.
6. the modified PVPP/TiO of cromoci Selective Separation in animal viscera according to claim 12It is nano combined Material, it is characterised in that: nano-TiO in the step (3)2The weight use of powder, modified PVPP, polyethylene glycol oxide and ferrocene Amount is than being 25-30:5-10:0.5-1:0.05-0.1.
7. the modified PVPP/TiO of cromoci Selective Separation in animal viscera according to claim 12It is nano combined Material, it is characterised in that: the operating condition of the microwave treater are as follows: rated frequency 2450MHz, input power 1300W, output Power 700W.
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