CN108440945A - A kind of preparation method of culture port sealing material - Google Patents
A kind of preparation method of culture port sealing material Download PDFInfo
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- CN108440945A CN108440945A CN201810199182.8A CN201810199182A CN108440945A CN 108440945 A CN108440945 A CN 108440945A CN 201810199182 A CN201810199182 A CN 201810199182A CN 108440945 A CN108440945 A CN 108440945A
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- 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
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Abstract
The invention discloses a kind of culture preparation methods of port sealing material, belong to technical field of polymer materials.It counts in parts by weight, 60~90 parts of N are weighed successively, N dimethylformamides, 20~25 parts of alkali lignins, 30~40 parts of polyethylene glycol, 10~15 parts of polyisocyanates, 3~6 parts of dibutyltindilaurylmercaptide cinnamic acids, 15~20 parts of modified vitrification micro-beads and 8~15 parts of additives, by alkali lignin and N, N dimethylformamides mix, and polyethylene glycol is added, polyisocyanates and dibutyltindilaurylmercaptide cinnamic acid, after being stirred, obtain blank, blank is mixed with modified vitrification micro-bead, and additive is added, after being stirred, blank must be pre-processed, pretreatment blank is laid in aluminium foil, and it is heating and curing, obtain thin slice, up to culture port sealing material.Gained culture of the invention has excellent permeability and bactericidal property with port sealing material.
Description
Technical field
The invention discloses a kind of culture preparation methods of port sealing material, belong to technical field of polymer materials.
Background technology
To prevent germ contamination, group culture container that from need to using joint filling material.Joint filling material constitutes closed with group culture container
Environment in container, also known as microenvironment have high relative humidity（RH）, low CO2Concentration（Illumination period is less than compensation point concentration）And height
C2H4The negative characteristics of concentration etc..Low CO2Concentration constrains the photosynthesis of tissue-cultured seedling in microenvironment；High C2H4Concentration inhibits tissue culture
The growth of seedling simultaneously causes early ageing；High RH reduces the respiration of tissue-cultured seedling and causes leaf development abnormal.Therefore, regulate and control microenvironment
The normal growth of tissue-cultured seedling is may advantageously facilitate, but the sterility requirements of microenvironment cause the difficulty of microenvironment direct regulation and control again,
Direct regulation and control is relatively difficult to achieve.
It is sealed using gas permeable material, promotes microenvironment（In container）Mass exchange between external environment（Such as steam, CO2
And C2H4）, it is a kind of regulation and control method of simple possible by adjusting external environment come indirect adjustments and controls microenvironment.Joint filling material gas permeability
It can play an important role to regulation process and its effect, Kozai etc. uses measurement indexs of the air penetrability E as permeability, E fixed
Justice is the rate of ventilation in unit hour group culture container.E values are the basic numbers for implementing microenvironment and quantifying and automating indirect adjustments and controls
According to measuring E values and the research of algorithm be of great significance.Kozai etc. first reported with CO2For search gas, using hand
Dynamic sampling and measuring method calculates air penetrability, and algorithm is using average estimation algorithm.Jeong etc. improves the measurement means of Kozai, but its
Algorithm does not have improvement.Ibaraki etc. is unable to control measurement error using steam as search gas.It is sealed for traditional port
The bad problem of bactericidal property and permeability existing for material also needs to study it.
Invention content
The present invention solves the technical problem of：It is bad for traditional port sealing material bactericidal property and permeability
The problem of, provide a kind of preparation method of culture port sealing material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）By glass bead and sodium hydroxide solution in mass ratio 1：5~1：8 mixing, impregnate, and filtering obtains alkalization glass bead,
It will alkalization glass bead and water in mass ratio 1：3~1：8 mixing, and the DOPA of 0.3~0.7 times of alkalization glass bead quality is added
Amine, after being stirred, filtering obtains pretreatment glass bead；
（2）It will pretreatment glass bead and graphene oxide mixture in mass ratio 1：5~1：8 mixing, impregnate, and filtering must filter
Cake, by filter cake and chitosan compound in mass ratio 1：5~1：6 mixing, impregnate, and filtering obtains pre- modified vitrification micro-bead；
（3）By pre- modified vitrification micro-bead and silver nitrate solution in mass ratio 1：3~1：8 mixing, impregnate, and filtering obtains filter residue, will filter
Slag and foaming agent in mass ratio 1：3~1：5 mixing, impregnate, and filtering obtains modified vitrification micro-bead；
（4）By sodium alginate and water in mass ratio 1：5~1：7 mixing, and the high iodine of 0.2~0.3 times of sodium alginate quality is added
Sour sodium, after being stirred, concentrated by rotary evaporation is dry, obtains modified sodium alginate；
（5）By modified sodium alginate and nano-titanium dioxide in mass ratio 3：1~5：1 mixing, obtains additive；
（6）It counts in parts by weight, weighs 60~90 parts of n,N-Dimethylformamide successively, 20~25 parts of alkali lignins, 30~40
Part polyethylene glycol, 10~15 parts of polyisocyanates, 3~6 parts of dibutyltindilaurylmercaptide cinnamic acids, 15~20 parts of modified vitrification micro-beads and 8
Alkali lignin is mixed with n,N-Dimethylformamide, and polyethylene glycol is added by~15 parts of additives, polyisocyanates and two fourths
Base tin tin dilaurate, after being stirred, obtains blank, blank is mixed, and additive is added with modified vitrification micro-bead, is stirred
Afterwards, pretreatment blank is obtained, pretreatment blank is laid in aluminium foil, and is heating and curing, obtains thin slice to get culture port sealing
Material.
Step（1）The grain size of the glass bead is 80~240 mesh.
Step（2）The preparation method of the graphene oxide mixture is by graphene oxide and water in mass ratio 1：300
~1：500 mixing, sonic oscillation must pre-process graphene oxide mixture, adjust the pH of pretreatment graphene oxide mixture,
Obtain graphene oxide mixture.
Step（2）The preparation method of the chitosan mixed liquor is by chitosan and water in mass ratio 1：120~1：150 is mixed
It closes, chitosan mixed liquor must be pre-processed, adjust pretreatment chitosan pH of mixed to 4.0~4.5, obtain chitosan mixed liquor.
Step（3）The foaming agent is n-hexane, any one in normal heptane or petroleum ether.
Step（6）The polyisocyanates is more phenylmethane polyisocyanates, methyl diphenylene diisocyanate or first
Any one in phenylene diisocyanate.
Step（6）The sheet thickness is 0.08~0.21mm.
The beneficial effects of the invention are as follows：
（1）Modified vitrification micro-bead is added when preparing culture port sealing material in the present invention, and first, glass bead is before modification
Basification, glass bead surface and internal micro- corruption are carried out, forming multi-through hole structure can be in foaming agent after being added in product
Synergistic effect under, multiple through-holes are formed on product, to make the gas permeability of product improve, secondly, glass bead is in modification
When processing, glass bead first under dopamine effect, forms positive charge, then be soaked in graphene oxide mixture on surface,
Since carboxylic acid group ionizes graphene oxide under alkaline condition so that graphene oxide becomes positively charged lotus, to aoxidize
Graphene can be combined with the glass bead with positive charge, after glass bead and graphene oxide impregnate, glass bead again with
Chitosan mixed liquid dipping, chitosan protonates in acid condition in chitosan mixed liquor, and chitosan surface becomes positively charged lotus,
Chitosan can be combined with graphene oxide, so as to form the complex protection of chitosan-graphene oxide on glass bead surface
Film, and then make product that there is excellent bactericidal effect；Also, the glass bead after immersion is mixed with silver nitrate solution, shell is poly-
The composite protection film of sugar-graphene oxide can fix silver ion, to make the anti-microbial property of product further increase；
（2）Additive is added when preparing culture port sealing material in the present invention, and additive is by modified sodium alginate and nanometer
Titanium dioxide is constituted, on the one hand, sodium alginate is after treatment, surface band aldehyde radical, so as to make modified sodium alginate add
After entering in product can with the hydroxy combining that contains on graphene oxide, so as to migrate nano-titanium dioxide to modified vitreous micro-
Near pearl, and then the bactericidal property of product is made to improve, on the other hand, the sodium alginate of addition contributes to the formation of film, to make
Product, which has, is easy molding.
Specific implementation mode
By graphene oxide and water in mass ratio 1：300~1：500 mixing, and by the mixture of graphene oxide and water with
Under conditions of power is 120~240W after 15~20min of sonic oscillation, graphene oxide mixture must be pre-processed, with quality point
The sodium hydroxide solution that number is 5~10% adjusts the pH to 6.8~7.5 of pretreatment graphene oxide mixture, obtains graphene oxide
Mixture, by chitosan and water in mass ratio 1：120~1：150 mixing are 45~55 DEG C in temperature, and rotating speed is 200~300r/
Under conditions of min, after being stirred 40~60min, chitosan mixed liquor must be pre-processed, the second for being 12~25% with mass fraction
Acid adjusts pretreatment chitosan pH of mixed to 4.0~4.5, obtains chitosan mixed liquor；It is 10 by glass bead and mass fraction
~18% sodium hydroxide solution in mass ratio 1：5~1：8 mixing, after impregnating 30~80min under room temperature, filtering obtains alkali
Change glass bead, by alkalization glass bead and water in mass ratio 1：3~1：8 mixing, and to alkalization glass bead and water mixing
The dopamine of 0.3~0.7 times of alkalization glass bead quality is added in object, is 40~45 DEG C in temperature, rotating speed is 250~350r/
After being stirred 20~45min under conditions of min, filtering obtains pretreatment glass bead；It will pretreatment glass bead and oxidation stone
Black alkene mixture in mass ratio 1：5~1：8 mixing, after temperature impregnates 35~80min under conditions of being 40~50 DEG C, filtering obtains
Filter cake, by filter cake and chitosan compound in mass ratio 1：5~1：6 mixing impregnate 40 under conditions of being 45~50 DEG C in temperature
After~50min, filtering obtains pre- modified vitrification micro-bead；By pre- modified vitrification micro-bead and silver nitrate solution in mass ratio 1：3~1：8
Mixing, after impregnating 60~100min under conditions of being 50~60 DEG C in temperature, filtering obtains filter residue, and filter residue and foaming agent are pressed matter
Measure ratio 1：3~1：5 mixing are 30~35 DEG C in temperature, rotating speed is stirred 30 under conditions of being 250~350r/min~
After 50min, filtering obtains modified vitrification micro-bead；By sodium alginate and water in mass ratio 1：5~1：7 are mixed in beaker, and to burning
The sodium metaperiodate of 0.2~0.3 times of sodium alginate quality is added in cup, is 40~50 DEG C in temperature, rotating speed is 300~400r/min
Under conditions of, after being stirred 30~60min, obtain sodium alginate mixture, by sodium alginate mixture in temperature be 60~80
DEG C, rotating speed is that 150~180r/min obtains concentrate under conditions of pressure is 500~600kPa after 30~55min of concentrated by rotary evaporation,
Under conditions of being 80~90 DEG C in temperature by concentrate after dry 25~35min, modified sodium alginate is obtained；By modified sodium alginate
With nano-titanium dioxide in mass ratio 3：1~5：1 mixing is 45~65 DEG C in temperature, and rotating speed is the condition of 200~300r/min
Under, it is stirred 5~10min, obtains additive；It counts in parts by weight, weighs 60~90 parts of n,N-Dimethylformamide successively, 20
~25 parts of alkali lignins, 30~40 parts of polyethylene glycol, 10~15 parts of polyisocyanates, 3~6 parts of dibutyltindilaurylmercaptide cinnamic acids, 15
Alkali lignin and n,N-Dimethylformamide are mixed in batch mixer by~20 parts of modified vitrification micro-beads and 8~15 parts of additives,
And polyethylene glycol is added into batch mixer, polyisocyanates and dibutyltindilaurylmercaptide cinnamic acid are 70~90 DEG C in temperature, and rotating speed is
After being stirred 30~45min under conditions of 200~350rmin, blank is obtained, blank and modified vitrification micro-bead are mixed in stirring
In machine, and additive is added into blender, is 80~90 DEG C in temperature, rotating speed stirs under conditions of being 200~300r/min
After mixing 15~30min, pretreatment blank is obtained, pretreatment blank is laid in aluminium foil, and the item for being 95~150 DEG C in temperature
After curing 30~40min under part, thin slice is obtained to get culture port sealing material.The grain size of the glass bead is 80~240
Mesh.The foaming agent is n-hexane, any one in normal heptane or petroleum ether.The polyisocyanates is more phenylmethane polyisocyanates
Any one in cyanate, methyl diphenylene diisocyanate or toluene di-isocyanate(TDI).The sheet thickness be 0.08~
0.21mm。
Example 1
By graphene oxide and water in mass ratio 1：500 mixing, and be 240W by the mixture of graphene oxide and water and power
Under conditions of after sonic oscillation 20min, graphene oxide mixture must be pre-processed, the sodium hydroxide for being 10% with mass fraction is molten
Liquid adjusts the pH to 7.5 of pretreatment graphene oxide mixture, obtains graphene oxide mixture, in mass ratio with water by chitosan
1：150 mixing are 55 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 60min, obtain pretreatment chitosan
Mixed liquor, the acetic acid for being 25% with mass fraction adjust pretreatment chitosan pH of mixed to 4.5, obtain chitosan mixed liquor；By glass
Change the sodium hydroxide solution in mass ratio 1 that microballon is 18% with mass fraction：8 mixing, after impregnating 80min under room temperature, mistake
Filter, obtains alkalization glass bead, by alkalization glass bead and water in mass ratio 1：8 mixing, and to the mixed of alkalization glass bead and water
The dopamine that 0.7 times of alkalization glass bead quality is added in object is closed, is 45 DEG C in temperature, rotating speed stirs under conditions of being 350r/min
After mixing mixing 45min, filtering obtains pretreatment glass bead；Pretreatment glass bead is pressed into quality with graphene oxide mixture
Than 1：8 mixing, after temperature impregnates 80min under conditions of being 50 DEG C, filtering obtains filter cake, and filter cake and chitosan compound are pressed matter
Measure ratio 1：6 mixing, after impregnating 50min under conditions of being 50 DEG C in temperature, filtering obtains pre- modified vitrification micro-bead；By pre- modified glass
Change microballon and silver nitrate solution in mass ratio 1：8 mixing, after impregnating 100min under conditions of being 60 DEG C in temperature, filtering must filter
Slag, by filter residue and foaming agent in mass ratio 1：5 mixing are 35 DEG C in temperature, and rotating speed is stirred under conditions of being 350r/min
After 50min, filtering obtains modified vitrification micro-bead；By sodium alginate and water in mass ratio 1：7 are mixed in beaker, and into beaker
The sodium metaperiodate of 0.3 times of sodium alginate quality is added, is 50 DEG C in temperature, under conditions of rotating speed is 400r/min, is stirred
After 60min, sodium alginate mixture is obtained, in temperature is 80 DEG C, rotating speed 180r/min by sodium alginate mixture, pressure is
Under conditions of 600kPa after concentrated by rotary evaporation 55min, concentrate is obtained, concentrate is dried into 35min under the conditions of at a temperature of 90 °C
Afterwards, modified sodium alginate is obtained；By modified sodium alginate and nano-titanium dioxide in mass ratio 5：1 mixing is 65 DEG C in temperature, turns
Under conditions of speed is 300r/min, it is stirred 10min, obtains additive；It counts in parts by weight, weighs 90 parts of N, N- diformazans successively
Base formamide, 25 parts of alkali lignins, 40 parts of polyethylene glycol, 15 parts of polyisocyanates, 6 parts of dibutyltindilaurylmercaptide cinnamic acids, 20 parts change
Property glass bead and 15 parts of additives, alkali lignin and n,N-Dimethylformamide are mixed in batch mixer, and to batch mixer
Middle addition polyethylene glycol, polyisocyanates and dibutyltindilaurylmercaptide cinnamic acid are 90 DEG C in temperature, and rotating speed is the condition of 350rmin
Under be stirred 45min after, obtain blank, blank and modified vitrification micro-bead be mixed in blender, and is added into blender
Additive is 90 DEG C in temperature, after rotating speed is stirred 30min under conditions of being 300r/min, obtains pretreatment blank, will locate in advance
Reason blank be laid in aluminium foil, and in temperature be 150 DEG C under conditions of solidification 40min after, it is close to get culture port to obtain thin slice
Closure material.The grain size of the glass bead is 240 mesh.The foaming agent is n-hexane.The polyisocyanates is more phenyl first
Alkane polyisocyanates.The sheet thickness is 0.21mm.
Example 2
By graphene oxide and water in mass ratio 1：500 mixing, and be 240W by the mixture of graphene oxide and water and power
Under conditions of after sonic oscillation 20min, graphene oxide mixture must be pre-processed, the sodium hydroxide for being 10% with mass fraction is molten
Liquid adjusts the pH to 7.5 of pretreatment graphene oxide mixture, obtains graphene oxide mixture, in mass ratio with water by chitosan
1：150 mixing are 55 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 60min, obtain pretreatment chitosan
Mixed liquor, the acetic acid for being 25% with mass fraction adjust pretreatment chitosan pH of mixed to 4.5, obtain chitosan mixed liquor；By glass
Change microballon and graphene oxide mixture in mass ratio 1：8 mixing, after temperature impregnates 80min under conditions of being 50 DEG C, filtering obtains
Filter cake, by filter cake and chitosan compound in mass ratio 1：6 mixing, after impregnating 50min under conditions of being 50 DEG C in temperature, mistake
Filter, obtains pre- modified vitrification micro-bead；By pre- modified vitrification micro-bead and silver nitrate solution in mass ratio 1：8 mixing, in temperature be 60 DEG C
Under conditions of impregnate 100min after, filtering, filter residue is obtained, by filter residue and foaming agent in mass ratio 1：5 mixing, in temperature be 35 DEG C,
After rotating speed is stirred 50min under conditions of being 350r/min, filtering obtains modified vitrification micro-bead；Sodium alginate and water are pressed into matter
Measure ratio 1：7 are mixed in beaker, and the sodium metaperiodate of 0.3 times of sodium alginate quality is added into beaker, are 50 DEG C in temperature, turn
Under conditions of speed is 400r/min, after being stirred 60min, sodium alginate mixture is obtained, by sodium alginate mixture in temperature
Be 80 DEG C, rotating speed 180r/min, pressure be 600kPa under conditions of after concentrated by rotary evaporation 55min, obtain concentrate, by concentrate in
Under the conditions of at a temperature of 90 °C after dry 35min, modified sodium alginate is obtained；Modified sodium alginate and nano-titanium dioxide are pressed into matter
Measure ratio 5：1 mixing is 65 DEG C in temperature, under conditions of rotating speed is 300r/min, is stirred 10min, obtains additive；By weight
Number meter, weighs 90 parts of n,N-Dimethylformamide successively, 25 parts of alkali lignins, 40 parts of polyethylene glycol, 15 parts of polyisocyanates,
6 parts of dibutyltindilaurylmercaptide cinnamic acids, 20 parts of modified vitrification micro-beads and 15 parts of additives, by alkali lignin and n,N-Dimethylformamide
It is mixed in batch mixer, and polyethylene glycol is added into batch mixer, polyisocyanates and dibutyltindilaurylmercaptide cinnamic acid are in temperature
90 DEG C, after rotating speed is stirred 45min under conditions of being 350rmin, blank is obtained, blank is mixed in modified vitrification micro-bead and is stirred
It mixes in machine, and additive is added into blender, be 90 DEG C in temperature, rotating speed is stirred under conditions of being 300r/min
After 30min, pretreatment blank is obtained, pretreatment blank is laid in aluminium foil, and is cured under conditions of being 150 DEG C in temperature
After 40min, thin slice is obtained to get culture port sealing material.The grain size of the glass bead is 240 mesh.The foaming agent is
N-hexane.The polyisocyanates is more phenylmethane polyisocyanates.The sheet thickness is 0.21mm.
Example 3
By graphene oxide and water in mass ratio 1：500 mixing, and be 240W by the mixture of graphene oxide and water and power
Under conditions of after sonic oscillation 20min, graphene oxide mixture must be pre-processed, the sodium hydroxide for being 10% with mass fraction is molten
Liquid adjusts the pH to 7.5 of pretreatment graphene oxide mixture, obtains graphene oxide mixture, in mass ratio with water by chitosan
1：150 mixing are 55 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 60min, obtain pretreatment chitosan
Mixed liquor, the acetic acid for being 25% with mass fraction adjust pretreatment chitosan pH of mixed to 4.5, obtain chitosan mixed liquor；By glass
Change the sodium hydroxide solution in mass ratio 1 that microballon is 18% with mass fraction：8 mixing, after impregnating 80min under room temperature, mistake
Filter, obtains alkalization glass bead, by alkalization glass bead and water in mass ratio 1：8 mixing, and to the mixed of alkalization glass bead and water
The dopamine that 0.7 times of alkalization glass bead quality is added in object is closed, is 45 DEG C in temperature, rotating speed stirs under conditions of being 350r/min
After mixing mixing 45min, filtering obtains pretreatment glass bead；It will pretreatment glass bead and silver nitrate solution in mass ratio 1：8 is mixed
It closes, after impregnating 100min under conditions of being 60 DEG C in temperature, filtering obtains filter residue, by filter residue and foaming agent in mass ratio 1：5 is mixed
It closes, is 35 DEG C in temperature, after rotating speed is stirred 50min under conditions of being 350r/min, filtering obtains modified vitrification micro-bead；It will
Sodium alginate and water in mass ratio 1：7 are mixed in beaker, and the periodic acid of 0.3 times of sodium alginate quality is added into beaker
Sodium is 50 DEG C in temperature, under conditions of rotating speed is 400r/min, after being stirred 60min, obtains sodium alginate mixture, will be extra large
Mosanom mixture is 80 DEG C, rotating speed 180r/min in temperature, under conditions of pressure is 600kPa after concentrated by rotary evaporation 55min,
Concentrate is obtained, concentrate after dry 35min, is obtained into modified sodium alginate under the conditions of at a temperature of 90 °C；It will modified alginic acid
Sodium and nano-titanium dioxide in mass ratio 5：1 mixing is 65 DEG C in temperature, under conditions of rotating speed is 300r/min, is stirred
10min obtains additive；It counts in parts by weight, weighs 90 parts of n,N-Dimethylformamide successively, 25 parts of alkali lignins, 40 parts poly-
Ethylene glycol, 15 parts of polyisocyanates, 6 parts of dibutyltindilaurylmercaptide cinnamic acids, 20 parts of modified vitrification micro-beads and 15 parts of additives, by alkali wood
Quality is mixed in n,N-Dimethylformamide in batch mixer, and polyethylene glycol is added into batch mixer, polyisocyanates and two
Butyl tin tin dilaurate is 90 DEG C in temperature, after rotating speed is stirred 45min under conditions of being 350rmin, blank is obtained, by base
Material is mixed in modified vitrification micro-bead in blender, and additive is added into blender, is 90 DEG C in temperature, rotating speed is
After being stirred 30min under conditions of 300r/min, pretreatment blank is obtained, pretreatment blank is laid in aluminium foil, and in temperature
Under conditions of degree is 150 DEG C after solidification 40min, thin slice is obtained to get culture port sealing material.The grain size of the glass bead
For 240 mesh.The foaming agent is n-hexane.The polyisocyanates is more phenylmethane polyisocyanates.The sheet thickness
For 0.21mm.
Example 4
By graphene oxide and water in mass ratio 1：500 mixing, and be 240W by the mixture of graphene oxide and water and power
Under conditions of after sonic oscillation 20min, graphene oxide mixture must be pre-processed, the sodium hydroxide for being 10% with mass fraction is molten
Liquid adjusts the pH to 7.5 of pretreatment graphene oxide mixture, obtains graphene oxide mixture, in mass ratio with water by chitosan
1：150 mixing are 55 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 60min, obtain pretreatment chitosan
Mixed liquor, the acetic acid for being 25% with mass fraction adjust pretreatment chitosan pH of mixed to 4.5, obtain chitosan mixed liquor；By glass
Change the sodium hydroxide solution in mass ratio 1 that microballon is 18% with mass fraction：8 mixing, after impregnating 80min under room temperature, mistake
Filter, obtains alkalization glass bead, by alkalization glass bead and water in mass ratio 1：8 mixing, and to the mixed of alkalization glass bead and water
The dopamine that 0.7 times of alkalization glass bead quality is added in object is closed, is 45 DEG C in temperature, rotating speed stirs under conditions of being 350r/min
After mixing mixing 45min, filtering obtains pretreatment glass bead；Pretreatment glass bead is pressed into quality with graphene oxide mixture
Than 1：8 mixing, after temperature impregnates 80min under conditions of being 50 DEG C, filtering obtains filter cake, and filter cake and chitosan compound are pressed matter
Measure ratio 1：6 mixing, after impregnating 50min under conditions of being 50 DEG C in temperature, filtering obtains pre- modified vitrification micro-bead；By sodium alginate
With water in mass ratio 1：7 are mixed in beaker, and the sodium metaperiodate of 0.3 times of sodium alginate quality is added into beaker, in temperature
It is 50 DEG C, under conditions of rotating speed is 400r/min, after being stirred 60min, obtains sodium alginate mixture, sodium alginate is mixed
Object is 80 DEG C, rotating speed 180r/min in temperature, under conditions of pressure is 600kPa after concentrated by rotary evaporation 55min, obtains concentrate, will
Concentrate after dry 35min, obtains modified sodium alginate under the conditions of at a temperature of 90 °C；By modified sodium alginate and nano-silica
Change titanium in mass ratio 5：1 mixing is 65 DEG C in temperature, under conditions of rotating speed is 300r/min, is stirred 10min, must add
Agent；It counts in parts by weight, weighs 90 parts of n,N-Dimethylformamide, 25 parts of alkali lignins, 40 parts of polyethylene glycol, more than 15 parts successively
Isocyanates, 6 parts of dibutyltindilaurylmercaptide cinnamic acids, 20 parts of pre- modified vitrification micro-beads and 15 parts of additives, by alkali lignin and N, N-
Dimethylformamide is mixed in batch mixer, and polyethylene glycol is added into batch mixer, polyisocyanates and dibutyltindilaurylmercaptide
Cinnamic acid is 90 DEG C in temperature, after rotating speed is stirred 45min under conditions of being 350rmin, blank is obtained, by blank and pre- modification
Glass bead is mixed in blender, and additive is added into blender, is 90 DEG C in temperature, rotating speed is the item of 300r/min
After being stirred 30min under part, pretreatment blank is obtained, pretreatment blank is laid in aluminium foil, and the item for being 150 DEG C in temperature
After curing 40min under part, thin slice is obtained to get culture port sealing material.The grain size of the glass bead is 240 mesh.It is described
Foaming agent is n-hexane.The polyisocyanates is more phenylmethane polyisocyanates.The sheet thickness is 0.21mm.
Example 5
By graphene oxide and water in mass ratio 1：500 mixing, and be 240W by the mixture of graphene oxide and water and power
Under conditions of after sonic oscillation 20min, graphene oxide mixture must be pre-processed, the sodium hydroxide for being 10% with mass fraction is molten
Liquid adjusts the pH to 7.5 of pretreatment graphene oxide mixture, obtains graphene oxide mixture, in mass ratio with water by chitosan
1：150 mixing are 55 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 60min, obtain pretreatment chitosan
Mixed liquor, the acetic acid for being 25% with mass fraction adjust pretreatment chitosan pH of mixed to 4.5, obtain chitosan mixed liquor；By glass
Change the sodium hydroxide solution in mass ratio 1 that microballon is 18% with mass fraction：8 mixing, after impregnating 80min under room temperature, mistake
Filter, obtains alkalization glass bead, by alkalization glass bead and water in mass ratio 1：8 mixing, and to the mixed of alkalization glass bead and water
The dopamine that 0.7 times of alkalization glass bead quality is added in object is closed, is 45 DEG C in temperature, rotating speed stirs under conditions of being 350r/min
After mixing mixing 45min, filtering obtains pretreatment glass bead；Pretreatment glass bead is pressed into quality with graphene oxide mixture
Than 1：8 mixing, after temperature impregnates 80min under conditions of being 50 DEG C, filtering obtains filter cake, and filter cake and chitosan compound are pressed matter
Measure ratio 1：6 mixing, after impregnating 50min under conditions of being 50 DEG C in temperature, filtering obtains pre- modified vitrification micro-bead；By pre- modified glass
Change microballon and silver nitrate solution in mass ratio 1：8 mixing, after impregnating 100min under conditions of being 60 DEG C in temperature, filtering must filter
Slag, by filter residue and foaming agent in mass ratio 1：5 mixing are 35 DEG C in temperature, and rotating speed is stirred under conditions of being 350r/min
After 50min, filtering obtains modified vitrification micro-bead；By sodium alginate and nano-titanium dioxide in mass ratio 5：1 mixes, and is in temperature
65 DEG C, under conditions of rotating speed is 300r/min, it is stirred 10min, obtains additive；It counts in parts by weight, weighs 90 parts successively
N,N-Dimethylformamide, 25 parts of alkali lignins, 40 parts of polyethylene glycol, 15 parts of polyisocyanates, 6 parts of dibutyltindilaurylmercaptide osmanthus
Alkali lignin and n,N-Dimethylformamide are mixed in batch mixer by acid, 20 parts of modified vitrification micro-beads and 15 parts of additives, and
Polyethylene glycol, polyisocyanates and dibutyltindilaurylmercaptide cinnamic acid are added into batch mixer, is 90 DEG C in temperature, rotating speed is
After being stirred 45min under conditions of 350rmin, blank is obtained, blank and modified vitrification micro-bead are mixed in blender, and to
Additive is added in blender, is 90 DEG C in temperature, after rotating speed is stirred 30min under conditions of being 300r/min, obtains pre- place
Manage blank, will pretreatment blank be laid in aluminium foil, and in temperature be 150 DEG C under conditions of solidification 40min after, obtain thin slice, i.e.,
Obtain culture port sealing material.The grain size of the glass bead is 240 mesh.The foaming agent is n-hexane.The polyisocyanate cyanogen
Acid esters is more phenylmethane polyisocyanates.The sheet thickness is 0.21mm.
Example 6
By graphene oxide and water in mass ratio 1：500 mixing, and be 240W by the mixture of graphene oxide and water and power
Under conditions of after sonic oscillation 20min, graphene oxide mixture must be pre-processed, the sodium hydroxide for being 10% with mass fraction is molten
Liquid adjusts the pH to 7.5 of pretreatment graphene oxide mixture, obtains graphene oxide mixture, in mass ratio with water by chitosan
1：150 mixing are 55 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 60min, obtain pretreatment chitosan
Mixed liquor, the acetic acid for being 25% with mass fraction adjust pretreatment chitosan pH of mixed to 4.5, obtain chitosan mixed liquor；By glass
Change the sodium hydroxide solution in mass ratio 1 that microballon is 18% with mass fraction：8 mixing, after impregnating 80min under room temperature, mistake
Filter, obtains alkalization glass bead, by alkalization glass bead and water in mass ratio 1：8 mixing, and to the mixed of alkalization glass bead and water
The dopamine that 0.7 times of alkalization glass bead quality is added in object is closed, is 45 DEG C in temperature, rotating speed stirs under conditions of being 350r/min
After mixing mixing 45min, filtering obtains pretreatment glass bead；Pretreatment glass bead is pressed into quality with graphene oxide mixture
Than 1：8 mixing, after temperature impregnates 80min under conditions of being 50 DEG C, filtering obtains filter cake, and filter cake and chitosan compound are pressed matter
Measure ratio 1：6 mixing, after impregnating 50min under conditions of being 50 DEG C in temperature, filtering obtains pre- modified vitrification micro-bead；By pre- modified glass
Change microballon and silver nitrate solution in mass ratio 1：8 mixing, after impregnating 100min under conditions of being 60 DEG C in temperature, filtering must filter
Slag, by filter residue and foaming agent in mass ratio 1：5 mixing are 35 DEG C in temperature, and rotating speed is stirred under conditions of being 350r/min
After 50min, filtering obtains modified vitrification micro-bead；By sodium alginate and water in mass ratio 1：7 are mixed in beaker, and into beaker
The sodium metaperiodate of 0.3 times of sodium alginate quality is added, is 50 DEG C in temperature, under conditions of rotating speed is 400r/min, is stirred
After 60min, sodium alginate mixture is obtained, in temperature is 80 DEG C, rotating speed 180r/min by sodium alginate mixture, pressure is
Under conditions of 600kPa after concentrated by rotary evaporation 55min, concentrate is obtained, concentrate is dried into 35min under the conditions of at a temperature of 90 °C
Afterwards, modified sodium alginate is obtained；It counts in parts by weight, weighs 90 parts of n,N-Dimethylformamide successively, 25 parts of alkali lignins, 40 parts
Polyethylene glycol, 15 parts of polyisocyanates, 6 parts of dibutyltindilaurylmercaptide cinnamic acids, 20 parts of modified vitrification micro-beads, by alkali lignin and N, N-
Dimethylformamide is mixed in batch mixer, and polyethylene glycol is added into batch mixer, polyisocyanates and dibutyltindilaurylmercaptide
Cinnamic acid is 90 DEG C in temperature, after rotating speed is stirred 45min under conditions of being 350rmin, obtains blank, blank is laid in aluminium
In foil, and in temperature be 150 DEG C under conditions of solidification 40min after, obtain thin slice to get culture port sealing material.The glass
The grain size for changing microballon is 240 mesh.The foaming agent is n-hexane.The polyisocyanates is more phenylmethane polyisocyanates.
The sheet thickness is 0.21mm.
Comparative example：The port sealing material of Haimen experiment equipment company production.
1 to 6 gained port sealing material of example and comparative example product are subjected to performance detection, specific detection method is as follows：
Its air penetrability is detected, and observes growth gesture, specific testing result is as shown in table 1：
Table 1：Performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example |
| Air penetrability/time h-1 | 1.586 | 1.341 | 1.328 | 1.408 | 1.315 | 1.325 | 1.204 |
| Growth potential | +++++ | +++ | +++ | ++++ | +++ | +++ | ++ |
It is best using the gas permeability and antibiotic property of 1 gained port sealing material of example, so the growth impetus is best.By above-mentioned detection
As a result it is found that present invention gained culture has excellent permeability and bactericidal property with port sealing material.
Claims (7)
1. a kind of preparation method of culture port sealing material, feature are being that specific preparation process is：
（1）By glass bead and sodium hydroxide solution in mass ratio 1：5~1：8 mixing, impregnate, and filtering obtains alkalization glass bead,
It will alkalization glass bead and water in mass ratio 1：3~1：8 mixing, and the DOPA of 0.3~0.7 times of alkalization glass bead quality is added
Amine, after being stirred, filtering obtains pretreatment glass bead；
（2）It will pretreatment glass bead and graphene oxide mixture in mass ratio 1：5~1：8 mixing, impregnate, and filtering must filter
Cake, by filter cake and chitosan compound in mass ratio 1：5~1：6 mixing, impregnate, and filtering obtains pre- modified vitrification micro-bead；
（3）By pre- modified vitrification micro-bead and silver nitrate solution in mass ratio 1：3~1：8 mixing, impregnate, and filtering obtains filter residue, will filter
Slag and foaming agent in mass ratio 1：3~1：5 mixing, impregnate, and filtering obtains modified vitrification micro-bead；
（4）By sodium alginate and water in mass ratio 1：5~1：7 mixing, and the high iodine of 0.2~0.3 times of sodium alginate quality is added
Sour sodium, after being stirred, concentrated by rotary evaporation is dry, obtains modified sodium alginate；
（5）By modified sodium alginate and nano-titanium dioxide in mass ratio 3：1~5：1 mixing, obtains additive；
（6）It counts in parts by weight, weighs 60~90 parts of n,N-Dimethylformamide successively, 20~25 parts of alkali lignins, 30~40
Part polyethylene glycol, 10~15 parts of polyisocyanates, 3~6 parts of dibutyltindilaurylmercaptide cinnamic acids, 15~20 parts of modified vitrification micro-beads and 8
Alkali lignin is mixed with n,N-Dimethylformamide, and polyethylene glycol is added by~15 parts of additives, polyisocyanates and two fourths
Base tin tin dilaurate, after being stirred, obtains blank, blank is mixed, and additive is added with modified vitrification micro-bead, is stirred
Afterwards, pretreatment blank is obtained, pretreatment blank is laid in aluminium foil, and is heating and curing, obtains thin slice to get culture port sealing
Material.
2. a kind of preparation method of culture port sealing material according to claim 1, it is characterised in that：Step（1）
The grain size of the glass bead is 80~240 mesh.
3. a kind of preparation method of culture port sealing material according to claim 1, it is characterised in that：Step（2）
The preparation method of the graphene oxide mixture is by graphene oxide and water in mass ratio 1：300~1：500 mixing, ultrasound
Oscillation must pre-process graphene oxide mixture, adjust the pH of pretreatment graphene oxide mixture, obtain graphene oxide mixing
Object.
4. a kind of preparation method of culture port sealing material according to claim 1, it is characterised in that：Step（2）
The preparation method of the chitosan mixed liquor is by chitosan and water in mass ratio 1：120~1：150 mixing, it is poly- must to pre-process shell
Sugared mixed liquor adjusts pretreatment chitosan pH of mixed to 4.0~4.5, obtains chitosan mixed liquor.
5. a kind of preparation method of culture port sealing material according to claim 1, it is characterised in that：Step（3）
The foaming agent is n-hexane, any one in normal heptane or petroleum ether.
6. a kind of preparation method of culture port sealing material according to claim 1, it is characterised in that：Step（6）
The polyisocyanates is more phenylmethane polyisocyanates, is appointed in methyl diphenylene diisocyanate or toluene di-isocyanate(TDI)
Meaning is a kind of.
7. a kind of preparation method of culture port sealing material according to claim 1, it is characterised in that：Step（6）
The sheet thickness is 0.08~0.21mm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628982A (en) * | 2015-02-13 | 2015-05-20 | 陕西科技大学 | Preparation method of alkali lignin-based waterborne polyurethane |
| CN106244084A (en) * | 2016-07-29 | 2016-12-21 | 合肥毅创钣金科技有限公司 | A kind of hollow glass micropearl strengthens the polyurethane foam glue of heat conductivity |
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2018
- 2018-03-12 CN CN201810199182.8A patent/CN108440945A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628982A (en) * | 2015-02-13 | 2015-05-20 | 陕西科技大学 | Preparation method of alkali lignin-based waterborne polyurethane |
| CN106244084A (en) * | 2016-07-29 | 2016-12-21 | 合肥毅创钣金科技有限公司 | A kind of hollow glass micropearl strengthens the polyurethane foam glue of heat conductivity |
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| Title |
|---|
| 宋启煌: "《绿色化工绿色生产工艺》", 31 March 2006, 广东科技出版社 * |
| 顾启胜: "《海藻酸盐生物医用材料与临床医学》", 30 April 2015, 上海科学技术出版社 * |
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