CN106905651A - The cromoci Selective Separation PVPP/TiO that is modified in animal viscera2Nano composite material - Google Patents

The cromoci Selective Separation PVPP/TiO that is modified in animal viscera2Nano composite material Download PDF

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CN106905651A
CN106905651A CN201710216766.7A CN201710216766A CN106905651A CN 106905651 A CN106905651 A CN 106905651A CN 201710216766 A CN201710216766 A CN 201710216766A CN 106905651 A CN106905651 A CN 106905651A
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pvpp
modified
tio
cromoci
nano
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CN106905651B (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 & Material Sciences (AREA)
  • 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 PVPP/TiO that is modified of cromoci Selective Separation in animal viscera2Nano composite material, is related to biomedicine technical field, specific preparation method to comprise the following steps：(1) nano-TiO2Powder is pre-processed, the preparation of (2) modified PVPP, and (3) are modified PVPP/TiO2The preparation of nano composite material.The made modified PVPP/TiO of the present invention2Nano composite material is exclusively used in the Selective Separation of cromoci in animal viscera, selectively reaches 85%, and adsorption efficiency is up to 89%, and the cromoci for being adsorbed is through Na3PO4Elution efficiency after eluant, eluent treatment reaches 95%, so as to realize that animal viscera acid carries efficiently separating for cromoci in solution, greatly improves the yield of cromoci.

Description

The cromoci Selective Separation PVPP/TiO that is modified in animal viscera2It is nano combined Material
Technical field：
The present invention relates to biomedicine technical field, and in particular to cromoci Selective Separation in a kind of animal viscera Use modified PVPP/TiO2Nano composite material.
Background technology：
Cromoci, is the electron transit mediator in biological oxidation process.Its action principle be in the presence of enzyme, To oxidation, the also original rapid rush enzyme effect organized.Usual exogenous cytochrome C can not enter healthy cell, but lack Membrane passage increases during oxygen, and cromoci is just likely to enter in cell and mitochondria, strengthens cellular oxidation, can carry The utilization of hyperoxia.Research shows, cromoci can be used in first aid and the adjuvant drug of histanoxia, such as anthracemia, Hypnotics poisoning, asphyxia neonatorum, serious shock anoxic, anesthesia and PUD D cause expiratory dyspnea, mountain hypoxia, brain lack Anoxic that oxygen, heart disease cause etc..
It is one of the approach for preparing cromoci to be isolated and purified from animal viscera.Because cromoci is a kind of stabilization Soluble protein, soluble in water, solubility is bigger in an acidic solution, therefore conventional acid solution is extracted.Using adsorptivity thing It is one of mode of quick separating cromoci that matter carries selective absorption cromoci in solution from acid, has adsorbed cytochromes The adsorbability material of C is eluted through eluant, eluent again, obtains the eluant, eluent containing cromoci.At present, have been reported that using artificial Zeolite has that the adsorption efficiency of institute adherent cell pigment C is low, elution efficiency is low after eluent as adsorbability material Problem, it is difficult to obtain the cromoci of high content, therefore need badly and develop adsorption efficiency and elution efficiency adsorptivity high Material.
The content of the invention：
The technical problems to be solved by the invention are that a kind of adsorption efficiency of offer and elution efficiency are high, selectivity is strong to be moved The cromoci Selective Separation PVPP/TiO that is modified in thing internal organs2Nano composite material.
The technical problems to be solved by the invention are realized using following technical scheme：
The cromoci Selective Separation PVPP/TiO that is modified in animal viscera2Nano composite material, specific preparation method Comprise the following steps：
(1) nano-TiO2Powder is pre-processed：To nano-TiO2Aromatic modified terpene resin and double fluoroforms are added in powder Sulfimide, after being sufficiently mixed with the programming rate of 5 DEG C/min be warming up to 70-80 DEG C insulation mixing 5-10min, then with 5 DEG C/ The cooling rate of min is cooled to 0-5 DEG C of insulation and stands 1-2h, is then warming up to 100-110 DEG C with the programming rate of 10 DEG C/min Insulation mixing 10-15min, is finally warming up to 500-550 DEG C of insulation roasting 2-3h；
(2) preparation of modified PVPP：To addition microcrystalline cellulose cross-linked polyacrylamide in PVPP And polyvinyl butyral resin, microwave treater microwave treatment 5-10min is utilized after being sufficiently mixed, add hexamethylol melamine Amine pregnancy ether, continues microwave treatment 3-5min, and be transferred to gained mixture in 0-5 DEG C of environment rapidly after terminating and seal by microwave treatment 0.5-1h is stood, 50-60 DEG C of warm water is then added under agitation, and reflux state is warming up to the programming rate of 5 DEG C/min and protected Temperature stirring 10-15min, after naturally cool to after room temperature will gained mixed solution send into spray dryer in, dry gained particle Micro mist is made through micronizer, modified PVPP is obtained final product；
(3) be modified PVPP/TiO2The preparation of nano composite material：To nano-TiO after pretreatment2Institute is added in powder The modified PVPP of system, utilizes microwave treater microwave treatment 5-10min, and 0.5- is stood in 15-20 DEG C of environment after being sufficiently mixed 1h, microwave treatment 3-5min, is subsequently adding polyethylene glycol oxide and ferrocene again, and microwave treatment 5- is continued after being well mixed 10min, in gained mixture sent into high energy ball mill after 45-50 DEG C, ground being obtained powdered changes Property PVPP/TiO2Nano composite material.
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 is modified in the step (1), and its specific preparation method is： Anthracene is dissolved in ethanol, terpene resin, HPO and titanate coupling agent is added, stirring makes it quiet after being uniformly dispersed 10-15min is put, and reflux state insulation mixing 0.5-1h is warming up to the programming rate of 5 DEG C/min, after naturally cool to 40- After 45 DEG C in feeding spray dryer, then to HPMA is added in dry gained particle, again with 5 DEG C/min's Programming rate is warming up to 120-125 DEG C of insulation mixing 0.5-1h, finally naturally cools to room temperature, obtains final product aromatic modified terpenes tree Fat.
The weight of the anthracene, ethanol, terpene resin, HPO, titanate coupling agent and HPMA is used Amount is than being 5-10:50-80:15-20:0.5-1:0.05-0.1:0.5-1.
PVPP, 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 PAMC in the step (2) Physical crosslinking is made, and its specific preparation method is：PAMC and poloxamer are dissolved in the water, and with 5 DEG C/ The programming rate of min is warming up to reflux state insulated and stirred 5-10min, adds microcrystalline cellulose and nanometer rubber powder, continues back Stream insulated and stirred 0.5-1h, is then cooled to 35-45 DEG C, the feeding freeze-drying of gained mixed liquor with the cooling rate of 10 DEG C/min In machine, dry gained solid and be made micro mist through micronizer, obtain final product microcrystalline cellulose cross-linked polyacrylamide.
The weight consumption ratio of the PAMC, poloxamer, water, microcrystalline cellulose and nanometer rubber powder is 5- 10:0.5-1:15-30:3-5:0.1-0.3。
Nano-TiO in the step (3)2Powder, the weight consumption ratio of modified PVPP, polyethylene glycol oxide and ferrocene are 25-30:5-10:0.5-1:0.05-0.1。
The condition of work of the microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
The beneficial effects of the invention are as follows：The made modified PVPP/TiO of the present invention2Nano composite material is exclusively used in animal viscera The Selective Separation of middle cromoci, carries out animal viscera acid and carries cell color in solution by being filled with being made after adsorption column The selective absorption of plain C, selectively reaches 85%, and adsorption efficiency is up to 89%, and the cromoci for being adsorbed is through Na3PO4 Elution efficiency after eluant, eluent treatment reaches 98%, so as to realize that animal viscera acid carries efficiently separating for cromoci in solution, Greatly improve the yield of cromoci.
Specific embodiment：
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
(1) nano-TiO2Powder is pre-processed：To 30 parts of nano-TiOs21 part of aromatic modified terpene resin and 0.3 are added in powder The double trifluoromethanesulfonimides of part, 70-80 DEG C of insulation mixing 10min is warming up to after being sufficiently mixed with the programming rate of 5 DEG C/min, 0-5 DEG C of insulation is cooled to the cooling rate of 5 DEG C/min again and stands 1h, 100- is then warming up to the programming rate of 10 DEG C/min 110 DEG C of insulation mixing 15min, are finally warming up to 500-550 DEG C of insulation roasting 3h；
(2) preparation of modified PVPP：To 1 part of microcrystalline cellulose crosslinked polypropylene of addition in 15 parts of PVPPs Acrylamide and 0.5 part of polyvinyl butyral resin, utilize microwave treater microwave treatment 5min after being sufficiently mixed, add 0.3 part Hexamethylolmelamine pregnancy ether, continues microwave treatment 5min, and gained mixture is transferred to 0-5 by microwave treatment rapidly after terminating Sealing and standing 1h in DEG C environment, then adds 50 parts of 50-60 DEG C of warm water, and heat up with the programming rate of 5 DEG C/min under agitation To reflux state insulated and stirred 15min, in gained mixed solution sent into spray dryer after room temperature, dry Gained particle is made micro mist through micronizer, obtains final product modified PVPP；
(3) be modified PVPP/TiO2The preparation of nano composite material：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 stood in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is subsequently adding 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene again, continues micro- after being well mixed Ripple process 5min, after naturally cool to after 45-50 DEG C by gained mixture send into high energy ball mill in, it is ground be obtained it is powdered Modified PVPP/TiO2Nano composite material.
The preparation of aromatic modified terpene resin：5 parts of anthracenes are dissolved in 80 parts of ethanol, 15 parts of terpene resins, 0.5 are added Part HPO and 0.05 part of titanate coupling agent, stirring make it that 15min is stood after being uniformly dispersed, and with the liter of 5 DEG C/min Warm speed is warming up to reflux state insulation mixing 1h, after naturally cool in sending into spray dryer after 40-45 DEG C, then to dry 0.5 part of HPMA is added in dry gained particle, 120-125 DEG C of guarantor is warming up to the programming rate of 5 DEG C/min again Temperature mixing 0.5h, finally naturally cools to room temperature, obtains final product aromatic modified terpene resin.
The preparation of microcrystalline cellulose cross-linked polyacrylamide：By 10 parts of PAMCs and 0.5 part of poloxamer It is dissolved in 30 parts of water, and reflux state insulated and stirred 10min is warming up to the programming rate of 5 DEG C/min, adds 5 parts of crystallites Cellulose and 0.1 part of nanometer rubber powder, continue the insulated and stirred 0.5h that flows back, and are then cooled to 35- with the cooling rate of 10 DEG C/min 45 DEG C, in gained mixed liquor feeding freeze drier, dry gained solid and be made micro mist through micronizer, obtain final product microcrystalline cellulose Plain cross-linked polyacrylamide.
Wherein, the condition of work of microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
Embodiment 2
(1) nano-TiO2Powder is pre-processed：To 35 parts of nano-TiOs21 part of aromatic modified terpene resin and 0.3 are added in powder The double trifluoromethanesulfonimides of part, 70-80 DEG C of insulation mixing 10min is warming up to after being sufficiently mixed with the programming rate of 5 DEG C/min, 0-5 DEG C of insulation is cooled to the cooling rate of 5 DEG C/min again and stands 1h, 100- is then warming up to the programming rate of 10 DEG C/min 110 DEG C of insulation mixing 15min, are finally warming up to 500-550 DEG C of insulation roasting 3h；
(2) preparation of modified PVPP：To 2 parts of microcrystalline cellulose crosslinked polypropylenes of addition in 15 parts of PVPPs Acrylamide and 0.5 part of polyvinyl butyral resin, utilize microwave treater microwave treatment 5min after being sufficiently mixed, add 0.3 part Hexamethylolmelamine pregnancy ether, continues microwave treatment 5min, and gained mixture is transferred to 0-5 by microwave treatment rapidly after terminating Sealing and standing 1h in DEG C environment, then adds 50 parts of 50-60 DEG C of warm water, and heat up with the programming rate of 5 DEG C/min under agitation To reflux state insulated and stirred 15min, in gained mixed solution sent into spray dryer after room temperature, dry Gained particle is made micro mist through micronizer, obtains final product modified PVPP；
(3) be modified PVPP/TiO2The preparation of nano composite material：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 stood in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is subsequently adding 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene again, continues micro- after being well mixed Ripple process 5min, after naturally cool to after 45-50 DEG C by gained mixture send into high energy ball mill in, it is ground be obtained it is powdered Modified PVPP/TiO2Nano composite material.
The preparation of aromatic modified terpene resin：5 parts of anthracenes are dissolved in 80 parts of ethanol, 20 parts of terpene resins, 0.5 are added Part HPO and 0.05 part of titanate coupling agent, stirring make it that 15min is stood after being uniformly dispersed, and with the liter of 5 DEG C/min Warm speed is warming up to reflux state insulation mixing 1h, after naturally cool in sending into spray dryer after 40-45 DEG C, then to dry 1 part of HPMA is added in dry gained particle, 120-125 DEG C of insulation is warming up to the programming rate of 5 DEG C/min again Mixing 0.5h, finally naturally cools to room temperature, obtains final product aromatic modified terpene resin.
The preparation of microcrystalline cellulose cross-linked polyacrylamide：By 10 parts of PAMCs and 0.5 part of poloxamer It is dissolved in 30 parts of water, and reflux state insulated and stirred 10min is warming up to the programming rate of 5 DEG C/min, adds 3 parts of crystallites Cellulose and 0.2 part of nanometer rubber powder, continue the insulated and stirred 0.5h that flows back, and are then cooled to 35- with the cooling rate of 10 DEG C/min 45 DEG C, in gained mixed liquor feeding freeze drier, dry gained solid and be made micro mist through micronizer, obtain final product microcrystalline cellulose Plain cross-linked polyacrylamide.
Wherein, the condition of work of microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
Reference examples 1
(1) nano-TiO2Powder is pre-processed：To 35 parts of nano-TiOs21 part of aromatic modified terpene resin and 0.3 are added in powder The double trifluoromethanesulfonimides of part, 70-80 DEG C of insulation mixing 10min is warming up to after being sufficiently mixed with the programming rate of 5 DEG C/min, 0-5 DEG C of insulation is cooled to the cooling rate of 5 DEG C/min again and stands 1h, 100- is then warming up to the programming rate of 10 DEG C/min 110 DEG C of insulation mixing 15min, are finally warming up to 500-550 DEG C of insulation roasting 3h；
(2) preparation of modified PVPP：To added in 15 parts of PVPPs 2 parts of PAMCs and 0.5 part of polyvinyl butyral resin, utilizes microwave treater microwave treatment 5min after being sufficiently mixed, add 0.3 part of hexamethylol Melamine pregnancy ether, continues microwave treatment 5min, and be transferred to gained mixture in 0-5 DEG C of environment rapidly after terminating by microwave treatment Sealing and standing 1h, then adds 50 parts of 50-60 DEG C of warm water, and be warming up to backflow shape with the programming rate of 5 DEG C/min under agitation State insulated and stirred 15min, after naturally cool to after room temperature will gained mixed solution send into spray dryer in, dry gained particle Micro mist is made through micronizer, modified PVPP is obtained final product；
(3) be modified PVPP/TiO2The preparation of nano composite material：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 stood in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is subsequently adding 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene again, continues micro- after being well mixed Ripple process 5min, after naturally cool to after 45-50 DEG C by gained mixture send into high energy ball mill in, it is ground be obtained it is powdered Modified PVPP/TiO2Nano composite material.
The preparation of aromatic modified terpene resin：5 parts of anthracenes are dissolved in 80 parts of ethanol, 20 parts of terpene resins, 0.5 are added Part HPO and 0.05 part of titanate coupling agent, stirring make it that 15min is stood after being uniformly dispersed, and with the liter of 5 DEG C/min Warm speed is warming up to reflux state insulation mixing 1h, after naturally cool in sending into spray dryer after 40-45 DEG C, then to dry 1 part of HPMA is added in dry gained particle, 120-125 DEG C of insulation is warming up to the programming rate of 5 DEG C/min again Mixing 0.5h, finally naturally cools to room temperature, obtains final product aromatic modified terpene resin.
Wherein, the condition of work of microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
Reference examples 2
(1) nano-TiO2Powder is pre-processed：To 35 parts of nano-TiOs21 part of terpene resin and 0.3 part of double trifluoro are added in powder Sulfonyl methane imines, after being sufficiently mixed with the programming rate of 5 DEG C/min be warming up to 70-80 DEG C insulation mixing 10min, then with 5 DEG C/ The cooling rate of min is cooled to 0-5 DEG C of insulation and stands 1h, is then warming up to 100-110 DEG C of guarantor with the programming rate of 10 DEG C/min Temperature mixing 15min, is finally warming up to 500-550 DEG C of insulation roasting 3h；
(2) preparation of modified PVPP：To 2 parts of microcrystalline cellulose crosslinked polypropylenes of addition in 15 parts of PVPPs Acrylamide and 0.5 part of polyvinyl butyral resin, utilize microwave treater microwave treatment 5min after being sufficiently mixed, add 0.3 part Hexamethylolmelamine pregnancy ether, continues microwave treatment 5min, and gained mixture is transferred to 0-5 by microwave treatment rapidly after terminating Sealing and standing 1h in DEG C environment, then adds 50 parts of 50-60 DEG C of warm water, and heat up with the programming rate of 5 DEG C/min under agitation To reflux state insulated and stirred 15min, in gained mixed solution sent into spray dryer after room temperature, dry Gained particle is made micro mist through micronizer, obtains final product modified PVPP；
(3) be modified PVPP/TiO2The preparation of nano composite material：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 stood in 15-20 DEG C of environment 0.5h, microwave treatment 5min, is subsequently adding 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene again, continues micro- after being well mixed Ripple process 5min, after naturally cool to after 45-50 DEG C by gained mixture send into high energy ball mill in, it is ground be obtained it is powdered Modified PVPP/TiO2Nano composite material.
The preparation of microcrystalline cellulose cross-linked polyacrylamide：By 10 parts of PAMCs and 0.5 part of poloxamer It is dissolved in 30 parts of water, and reflux state insulated and stirred 10min is warming up to the programming rate of 5 DEG C/min, adds 3 parts of crystallites Cellulose and 0.2 part of nanometer rubber powder, continue the insulated and stirred 0.5h that flows back, and are then cooled to 35- with the cooling rate of 10 DEG C/min 45 DEG C, in gained mixed liquor feeding freeze drier, dry gained solid and be made micro mist through micronizer, obtain final product microcrystalline cellulose Plain cross-linked polyacrylamide.
Wherein, the condition of work of microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
Reference examples 3
(1) preparation of modified PVPP：To 2 parts of microcrystalline cellulose crosslinked polypropylenes of addition in 15 parts of PVPPs Acrylamide and 0.5 part of polyvinyl butyral resin, utilize microwave treater microwave treatment 5min after being sufficiently mixed, add 0.3 part Hexamethylolmelamine pregnancy ether, continues microwave treatment 5min, and gained mixture is transferred to 0-5 by microwave treatment rapidly after terminating Sealing and standing 1h in DEG C environment, then adds 50 parts of 50-60 DEG C of warm water, and heat up with the programming rate of 5 DEG C/min under agitation To reflux state insulated and stirred 15min, in gained mixed solution sent into spray dryer after room temperature, dry Gained particle is made micro mist through micronizer, obtains final product modified PVPP；
(2) be modified PVPP/TiO2The preparation of nano composite material：To 30 parts of nano-TiOs25 parts of addition is made modified in powder PVPP, utilizes microwave treater microwave treatment 5min after being sufficiently mixed, and 0.5h is stood in 15-20 DEG C of environment, again microwave Treatment 5min, is subsequently adding 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, and microwave treatment 5min is continued after being well mixed, and treats It is ground that powdered modified PVPP/ is obtained during gained mixture sent into high energy ball mill after naturally cooling to 45-50 DEG C TiO2Nano composite material.
The preparation of microcrystalline cellulose cross-linked polyacrylamide：By 10 parts of PAMCs and 0.5 part of poloxamer It is dissolved in 30 parts of water, and reflux state insulated and stirred 10min is warming up to the programming rate of 5 DEG C/min, adds 3 parts of crystallites Cellulose and 0.2 part of nanometer rubber powder, continue the insulated and stirred 0.5h that flows back, and are then cooled to 35- with the cooling rate of 10 DEG C/min 45 DEG C, in gained mixed liquor feeding freeze drier, dry gained solid and be made micro mist through micronizer, obtain final product microcrystalline cellulose Plain cross-linked polyacrylamide.
Wherein, the condition of work of microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
Reference examples 4
Modified PVPP/TiO2The preparation of nano composite material：To 30 parts of nano-TiOs25 parts of crosslinked polyethylenes are added in powder Pyrrolidones, utilizes microwave treater microwave treatment 5min after being sufficiently mixed, and 0.5h is stood in 15-20 DEG C of environment, again Microwave treatment 5min, is subsequently adding 0.5 part of polyethylene glycol oxide and 0.05 part of ferrocene, and microwave treatment is continued after being well mixed 5min, after naturally cool to, by gained mixture feeding high energy ball mill, ground prepared powdered is modified after 45-50 DEG C PVPP/TiO2Nano composite material.
Wherein, the condition of work of microwave treater is：Rated frequency 2450MHz, input power 1300W, power output 700W。
Embodiment 3
It is utilized respectively equivalent embodiment 1, embodiment 2, reference examples 1, reference examples 2, reference examples 3 and reference examples 4 made modified PVPP/TiO2Nano composite material carries out the Selective Separation of cromoci to carrying solution with batch equivalent Pigs Hearts acid, and setting makes Use equivalent nano-TiO2Powder is directly separated cromoci as reference examples 5, then using 0.1mol/LNa3PO4Eluant, eluent is to inhaling Attached cromoci is eluted, while Selective Separation effect is measured, as a result as shown in table 1.
The Pigs Hearts acid of table 1 puies forward the Selective Separation effect of cromoci in solution
Project 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
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The technology of the industry Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and its Equivalent thereof.

Claims (9)

1. in animal viscera cromoci Selective Separation with modified PVPP/TiO2Nano composite material, it is characterised in that specific Preparation method comprises the following steps：
(1) nano-TiO2Powder is pre-processed：To nano-TiO2Aromatic modified terpene resin and double fluoroform sulphonyl are added in powder Imines, 70-80 DEG C of insulation mixing 5-10min is warming up to after being sufficiently mixed with the programming rate of 5 DEG C/min, then with 5 DEG C/min's Cooling rate is cooled to 0-5 DEG C of insulation and stands 1-2h, and it is mixed to be then warming up to 100-110 DEG C of insulation with the programming rate of 10 DEG C/min 10-15min is closed, 500-550 DEG C of insulation roasting 2-3h is finally warming up to；
(2) preparation of modified PVPP：To adding microcrystalline cellulose cross-linked polyacrylamide and poly- in PVPP Vinyl butyral, utilizes microwave treater microwave treatment 5-10min after being sufficiently mixed, add hexamethylolmelamine six Methyl ether, continues microwave treatment 3-5min, and microwave treatment is rapid after terminating to be transferred to sealing and standing in 0-5 DEG C of environment by gained mixture 0.5-1h, then adds 50-60 DEG C of warm water, and is warming up to reflux state insulation with the programming rate of 5 DEG C/min and stir under agitation 10-15min is mixed, is surpassed after naturally cool to after room temperature gained particle warp in gained mixed solution feeding spray dryer, will be dried Atomizer is made micro mist, obtains final product modified PVPP；
(3) be modified PVPP/TiO2The preparation of nano composite material：To nano-TiO after pretreatment2Made changing is added in powder Property PVPP, microwave treater microwave treatment 5-10min is utilized after being sufficiently mixed, and 0.5-1h is stood in 15-20 DEG C of environment, then Secondary microwave treatment 3-5min, is subsequently adding polyethylene glycol oxide and ferrocene, and microwave treatment 5-10min is continued after being well mixed, and treats It is ground that powdered modified PVPP/ is obtained during gained mixture sent into high energy ball mill after naturally cooling to 45-50 DEG C TiO2Nano composite material.
2. in animal viscera according to claim 1 cromoci Selective Separation with modified PVPP/TiO2It 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. in animal viscera according to claim 1 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：Aromatic modified terpene resin is formed by terpene resin through anthracene is modified in the step (1), its specific system Preparation Method is：Anthracene is dissolved in ethanol, terpene resin, HPO and titanate coupling agent is added, stirring makes its point Uniform rear standing 10-15min is dissipated, and reflux state insulation mixing 0.5-1h is warming up to the programming rate of 5 DEG C/min, treat nature After being cooled to 40-45 DEG C send into spray dryer in, then to dry gained particle in add HPMA, again with The programming rate of 5 DEG C/min is warming up to 120-125 DEG C of insulation mixing 0.5-1h, finally naturally cools to room temperature, obtains final product aromatic hydrocarbons and changes Property terpene resin.
4. in animal viscera according to claim 3 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：The anthracene, ethanol, terpene resin, HPO, titanate coupling agent and HPMA Weight consumption ratio be 5-10:50-80:15-20:0.5-1:0.05-0.1:0.5-1.
5. in animal viscera according to claim 1 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：PVPP, 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。
6. in animal viscera according to claim 1 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：Microcrystalline cellulose cross-linked polyacrylamide is by microcrystalline cellulose and cation poly- third in the step (2) Acrylamide is made through physical crosslinking, and its specific preparation method is：PAMC and poloxamer are dissolved in the water, And reflux state insulated and stirred 5-10min is warming up to the programming rate of 5 DEG C/min, add microcrystalline cellulose and nanometre glue Powder, continues the insulated and stirred 0.5-1h that flows back, and is then cooled to 35-45 DEG C with the cooling rate of 10 DEG C/min, and gained mixed liquor send Enter in freeze drier, dry gained solid and be made micro mist through micronizer, obtain final product microcrystalline cellulose cross-linked polyacrylamide.
7. in animal viscera according to claim 6 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：The weight of the PAMC, poloxamer, water, microcrystalline cellulose and nanometer rubber powder is used Amount is than being 5-10:0.5-1:15-30:3-5:0.1-0.3.
8. in animal viscera according to claim 1 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：Nano-TiO in the step (3)2Powder, the weight of modified PVPP, polyethylene glycol oxide and ferrocene are used Amount is than being 25-30:5-10:0.5-1:0.05-0.1.
9. in animal viscera according to claim 1 cromoci Selective Separation with modified PVPP/TiO2It is nano combined Material, it is characterised in that：The condition of work of the microwave treater is：Rated frequency 2450MHz, input power 1300W, output Power 700W.
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EP0927572A2 (en) * 1997-12-30 1999-07-07 Kolon Industries, Inc. A polysulfone based hollow fiber membrane, and a process for preparing the same
CN1921929A (en) * 2004-02-19 2007-02-28 门布拉内有限公司 High-flux dialysis membrane with an improved separation behavior
CN1921930A (en) * 2004-02-19 2007-02-28 门布拉内有限公司 Dialysis membrane having improved average molecular distance
WO2014092660A1 (en) * 2012-12-13 2014-06-19 Istem Medikal Tibbi Cihaz Ve Sanayi Limited Sirketi A ready for use hydrophilic catheter set that does not lose its lubricious efficiency when left in water for a extended period of time, with increased lubricious characteristics, and a production method for this catheter set

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1117979A (en) * 1994-06-01 1996-03-06 埃勒夫阿托化学有限公司 Stable aqueous dispersive body of hydroxyleste fluoridated copolymer and acrylic copolymer and preparation and application as aqueous pait of same
EP0927572A2 (en) * 1997-12-30 1999-07-07 Kolon Industries, Inc. A polysulfone based hollow fiber membrane, and a process for preparing the same
CN1921929A (en) * 2004-02-19 2007-02-28 门布拉内有限公司 High-flux dialysis membrane with an improved separation behavior
CN1921930A (en) * 2004-02-19 2007-02-28 门布拉内有限公司 Dialysis membrane having improved average molecular distance
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