CN105542204B - A kind of preparation method of monocycle oxygen terminated polysiloxane modified gelatin parents' film - Google Patents
A kind of preparation method of monocycle oxygen terminated polysiloxane modified gelatin parents' film Download PDFInfo
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- 108010010803 Gelatin Proteins 0.000 title claims abstract description 104
- 229920000159 gelatin Polymers 0.000 title claims abstract description 104
- 239000008273 gelatin Substances 0.000 title claims abstract description 104
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 104
- 235000011852 gelatine desserts Nutrition 0.000 title claims abstract description 104
- -1 polysiloxane Polymers 0.000 title claims abstract description 86
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 64
- 239000001301 oxygen Substances 0.000 title claims abstract description 60
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 60
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 406
- 238000001035 drying Methods 0.000 claims abstract description 109
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 238000003756 stirring Methods 0.000 claims abstract description 51
- 235000019441 ethanol Nutrition 0.000 claims description 202
- 108010025899 gelatin film Proteins 0.000 claims description 113
- 239000010802 sludge Substances 0.000 claims description 82
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 40
- 229910052708 sodium Inorganic materials 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 22
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims 12
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims 9
- 239000000243 solution Substances 0.000 abstract description 113
- 230000002209 hydrophobic effect Effects 0.000 abstract description 24
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 250
- 229960004756 ethanol Drugs 0.000 description 196
- 239000007789 gas Substances 0.000 description 125
- 238000000034 method Methods 0.000 description 106
- 239000010985 leather Substances 0.000 description 10
- 230000008859 change Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 230000005311 nuclear magnetism Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 4
- 239000004475 Arginine Substances 0.000 description 3
- 239000004472 Lysine Substances 0.000 description 3
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 3
- 229910018540 Si C Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 3
- 238000005034 decoration Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 102000008186 Collagen Human genes 0.000 description 2
- 108010035532 Collagen Proteins 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 229920001436 collagen Polymers 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001184 polypeptide Polymers 0.000 description 2
- 102000004196 processed proteins & peptides Human genes 0.000 description 2
- 108090000765 processed proteins & peptides Proteins 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000010539 anionic addition polymerization reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- 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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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Jellies, Jams, And Syrups (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Medicinal Preparation (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to a kind of preparation methods of monocycle oxygen terminated polysiloxane modified gelatin parents' film, Gelatin Yu Shuizhong is configured to the aqueous solution that mass concentration is 3 ~ 8%, under conditions of 40~60 DEG C, pH are 8~11, Surfactant SDS is added, after stirring 4~8 hours, solution is divided into the monocycle oxygen terminated polysiloxane for being added that molecular weight is 500 in 4 parts, first part, obtains solution A;Second part is added the monocycle oxygen terminated polysiloxane that molecular weight is 1000, obtains solution B;The monocycle oxygen terminated polysiloxane that molecular weight is 2000 is added in third part, obtains solution C;4th part is added without monocycle oxygen terminated polysiloxane, for solution D, wherein A, B, the dosage of monocycle oxygen terminated polysiloxane is 0.04~3.0 times of gelatin mole in C solution, A, B, C, after tetra- mixed solutions of D the reaction was continued at 40~60 DEG C 24~30h, it is (1~5): (1~5): (1~5) by adjusting four kinds of solution mixed proportions: after 1, measures 5~10g solution and be placed in mold, dehydrated alcohol is added, in 25~70 DEG C of normal pressure drying in oven, parents' film that one side is hydrophilic, another side is hydrophobic is obtained, the film ductility is good, soft.
Description
Technical field
The present invention relates to parents' film, in particular to a kind of preparation side of monocycle oxygen terminated polysiloxane modified gelatin parents' film
Method.This parents' film have one side it is hydrophilic, while hydrophobic, the features such as ductility is good, and film is soft, removed from office be especially suitable for suitcase,
The finishing agent of clothing leather or car decoration leather.
Background technique
Gelatin is obtained from the by-product or waste of cheap process hides, pharmacy and food, is a kind of renewable
Resource has biological degradability, and there are no pollution to the environment.Gelatin has become the important raw material for preparing protein film, such as other
Natural macromolecular material is the same, after this kind of protein material film forming, there are plastic senses it is strong, water-resistance and rotproofness are poor the problems such as.Silicon
Siloxane modified gelatin can improve the water-resistance and flexibility [201310012009.X] of gelatin film to a certain extent, but silicon
Disorder distribution of the oxygen alkane component in film directly affects membrane structure, film properties and film application.
Parents' film can make silicone components be distributed in the one side of film, and another side is gelatin, to make the property of membrane material
Two kinds of properties are also presented in matter and function.The present invention passes through Macromolecular self-assembly mistake for using the interaction between each macromolecular
Journey prepares novel gelatin parents film.
Summary of the invention
The purpose of the present invention is overcoming above-mentioned deficiency, the preparation of monocycle oxygen terminated polysiloxane modified gelatin parents' film is provided
Method, invention preparation have the characteristics that strong gelatin leather finishing agent hydrophobic, ductility is good, thermal stability is low, film is soft.
The technical scheme adopted by the invention is as follows:
A kind of preparation method of monocycle oxygen terminated polysiloxane modified gelatin parents' film, comprises the following steps that
(1) Gelatin Yu Shuizhong being configured to aqueous solution, adjusts its temperature at 40~60 DEG C, regulation system pH is 8~
11, mass concentration is 3~8%, and solution is divided into 4 equal portions, and sodium alkyl sulfate is all added into every portion, stirs 4~8h, wherein
The long alkyl chains of sodium alkyl sulfate are 10,12,14 or 16, and dosage is the 1~20% of gelatin quality;
(2) solution for obtaining step (1) takes out a, and the list that point 1~8 batch of addition molecular weight is 500 is epoxy-capped poly-
Siloxanes, the dosage of monocycle oxygen terminated polysiloxane are 0.04~3.0 times of primary amine groups mole in gelatin molecule, in 40~
60 DEG C of 24~30h of reaction, obtain solution A, and wherein concentration of polymer solution is 1 ~ 30%;
(3) solution for obtaining step (1) takes out a, and the epoxy-capped poly- silicon oxygen of list that molecular weight is 1000 is added portionwise
Alkane, the dosage of monocycle oxygen terminated polysiloxane is 0.04~3.0 times of primary amine groups mole in gelatin molecule, in 40~60 DEG C
24~30h is reacted, solution A is obtained, wherein concentration of polymer solution is 1 ~ 30%;
(4) solution for obtaining step (1) takes out a, and the epoxy-capped poly- silicon oxygen of list that molecular weight is 2000 is added portionwise
Alkane, the dosage of monocycle oxygen terminated polysiloxane is 0.04~3.0 times of primary amine groups mole in gelatin molecule, in 40~60 DEG C
24~30h is reacted, solution A is obtained, wherein concentration of polymer solution is 1 ~ 30%;
(5) solution obtained step (1) takes out a, in 40~70 DEG C of persistently stirrings 12~for 24 hours, obtains solution D,
Middle solution concentration is 1~10%;
(6) by solution A, solution B, solution C and solution D with mass ratio be (1~5): (1~5): (1~5): 1 ratio mix
Afterwards, it obtains containing the polysiloxane-modified gelatin mixed aqueous solution of different weight average molecular weight;
(7) it weighs 5~10g and contains the different polysiloxane-modified gelatin mixed aqueous solutions of weight average molecular weight, be placed in polytetrafluoro
In the mold of ethylene, it is added dehydrated alcohol in a mold, the volume ratio of ethyl alcohol and mixed liquor is 1:(1~8), after mixing,
It is dried in 25~70 DEG C of room temperature baking oven, obtains the modified gelatin film with different contact angles, can be obtained under part of ratio
Parents' film hydrophobic while hydrophilic is obtained, the film ductility is good.
The present invention has following remarkable advantage using the monocycle oxygen terminated polysiloxane modified gelatin of different molecular weight: first
First, the longer monocycle oxygen terminated polysiloxane modified gelatin of molecule segment can form microphase-separated with gelatin molecule, promote material
Embody excellent, special performance.Firstly, monocycle oxygen terminated polysiloxane is incompatible with gelatin, the two is led in film forming procedure
It crosses intermolecular interaction and forms micro phase separation structure, material is promoted to embody excellent, special performance.Secondly, siloxanes group
Change of gradient is presented in point content in the longitudinal direction, makes the two sides of film that heterogeneity be presented, and is on one side gelatin enrichment, can be tight with hide
Close combination;Another side is siloxanes enrichment, and siloxanes is one kind using duplicate Si-O key as main chain, has been directly connected on silicon atom
The polymer of machine group;This special construction of organosilicon and composition, having it, low-temperature flexibility is good, surface tension is low, biological
The features such as compatibility is good, resistance to combustion, good weatherability, water-tolerant, thermostabilization are good and good permeability.Third, silicone components are in film
In be orderly distributed, so that film is had the characteristics that softness, meet suitcase leather, clothing leather or car decoration leather high demand.In exploration
Can superior, cheap hybrid protein finishing agent while, prepare novel gelatin membrane material, obtain the waste of leather industry
To high level conversion.
Monocycle oxygen terminated polysiloxane modified gelatin parents' film of different molecular weight of the present invention can be used as suitcase leather,
The finishing agent of clothing leather or car decoration leather.
Detailed description of the invention
Fig. 1 is the infrared spectrum of gelatin;
Fig. 2 is the infrared spectrum of monocycle oxygen terminated polysiloxane grafted gelatin of the present invention;
Fig. 3 is the gas/liquid face of parents' film of the present invention, solid-liquid face contact angle photo;
Fig. 4 is the energy dispersion spectrogram of parents' film of the present invention.
Specific embodiment:
Carry out the present invention is described in detail below by specific embodiment:
Primary amino group content measures [ using the method for patent CN102393466A ] with primary amino radical tester in gelatin molecule;
Monocycle oxygen terminated polysiloxane is synthesized with anionic polymerization;
Polymer architecture is with nuclear-magnetism, infrared, x-ray photoelectron spectroscopy characterization;
Contact angle is measured with contact angle instrument;
Glass transition temperature (Tg) is with the measurement of differential thermal calorimetric scan instrument;
Viscosity is with rotary viscosity design determining;
Elemental analysis is with scanning electron microscope-energy dispersive spectrum integrated instrument measurement.
Embodiment 1:
5 grams of gelatin are added in three mouthfuls of reaction flasks equipped with thermometer socket, sample tap and condenser socket and (account for gross mass
5%), 95 grams of deionized waters are heated with stirring to 50 DEG C, after gelatin is completely dissolved, be added 0.65mL2 mol/L hydroxide
Sodium, adjusting reaction pH is 10.0, is added 0.3g sodium alkyl sulfonate (account for gelatin quality 6%), continues stirring to dodecyl sodium sulfonate
It is continuous or monocycle oxygen terminated polysiloxane (Mw=500) is added portionwise after sodium is completely dissolved, monocycle oxygen terminated polysiloxane with it is bright
The molar ratio of glue is 0.8:1, and reaction starts, and the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring
And heating, obtain monocycle oxygen terminated polysiloxane modified gelatin solution (solution A).
Viscosity is 700 centipoises at 50 DEG C of above-mentioned feed liquid, is placed 48 hours at room temperature, and film is formed, and 40 DEG C dry 6 hours,
Moisture removal is further removed, film flexible is formed, raw material gelatin filmT gIt is 215.7 DEG C, having for modified gelatin film is doubleT g,
For 175 DEG C and 220 DEG C;Nuclear-magnetism shows that lysine, γ-C signal disappears on arginine molecule, and the peak of organosilicon Si-C is formed;
XPS shows that the chemical shift of N moves to 399.96, shows that C-N is formed.
5 grams of gelatin are added in three mouthfuls of reaction flasks equipped with thermometer socket, sample tap and condenser socket and (account for gross mass
5%), 95 grams of deionized waters are heated with stirring to 50 DEG C, after gelatin is completely dissolved, be added 0.65mL2 mol/L hydroxide
Sodium, adjusting reaction pH is 10.0, is added 0.3g sodium alkyl sulfonate (account for gelatin quality 6%), continues stirring to dodecyl sodium sulfonate
It is continuous or monocycle oxygen terminated polysiloxane (Mw=1000) is added portionwise after sodium is completely dissolved, monocycle oxygen terminated polysiloxane with it is bright
The molar ratio of glue is 0.8:1, and reaction starts, and the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring
And heating, obtain monocycle oxygen terminated polysiloxane modified gelatin solution (solution B).
There are 3 collagen polypeptide infrared lights in the infrared spectrogram (Fig. 2) of monocycle oxygen terminated polysiloxane modified gelatin
The new bands of a spectrum not having in spectrogram, their ownership are as follows: (1) 802cm-1The peak that place occurs is Si-CH3The rocking vibration of middle C-H
Absorption peak, this is one of characteristic peak of polysiloxanes;(2)1261cm-1The peak that place occurs is Si-CH3The symmetric deformation of middle C-H is curved
Bent vibration absorption peak, this is also one of characteristic peak of polysiloxanes;(3)2963cm-1The stretching vibration that the peak that place occurs is C-H is inhaled
It receives peak and passes through 3 Si-CH occurred in spectrogram3Characteristic absorption peak, the epoxy group in the epoxy-capped polysiloxanes of instruction sheet
It is reacted with the primary amino group on collagen polypeptide.
Above-mentioned viscosity of sludge is 800 centipoises (50 DEG C), is placed 48 hours at room temperature, and film is formed, and 40 DEG C dry 6 hours,
Moisture removal is further removed, film flexible is formed, raw material gelatin filmT g It is 215.7 DEG C, having for modified gelatin film is doubleT g,
For 205 DEG C and 220 DEG C;Nuclear-magnetism shows that lysine, γ-C signal disappears on arginine molecule, and the peak of organosilicon Si-C is formed;
XPS shows that the chemical shift of N moves to 399.87, shows that C-N is formed.
5 grams of gelatin are added in three mouthfuls of reaction flasks equipped with thermometer socket, sample tap and condenser socket and (account for gross mass
5%), 95 grams of deionized waters are heated with stirring to 50 DEG C, after gelatin is completely dissolved, be added 0.65mL2 mol/L hydroxide
Sodium, adjusting reaction pH is 10.0, is added 0.3g sodium alkyl sulfonate (account for gelatin quality 6%), continues stirring to dodecyl sodium sulfonate
It is continuous or monocycle oxygen terminated polysiloxane (Mw=2000) is added portionwise after sodium is completely dissolved, monocycle oxygen terminated polysiloxane with it is bright
The molar ratio of glue is 0.8:1, and reaction starts, and the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring
And heating, obtain monocycle oxygen terminated polysiloxane modified gelatin solution (solution C).
Above-mentioned viscosity of sludge is 850 centipoises (50 DEG C), is placed 48 hours at room temperature, and film is formed, and 40 DEG C dry 6 hours,
Moisture removal is further removed, film flexible is formed, the Tg of raw material gelatin film is 215.7 DEG C, and the Tg of modified gelatin film is 170
℃;Nuclear-magnetism shows that lysine, γ-C signal disappears on arginine molecule, and the peak of organosilicon Si-C is formed;XPS shows the chemistry of N
Displacement moves to 399.56, shows that C-N is formed.
5 grams of gelatin are added in three mouthfuls of reaction flasks equipped with thermometer socket, sample tap and condenser socket and (account for gross mass
5%), 95 grams of deionized waters are heated with stirring to 50 DEG C, after gelatin is completely dissolved, be added 0.65mL2 mol/L hydroxide
Sodium, adjusting reaction pH is 10.0, is added 0.3g sodium alkyl sulfonate (account for gelatin quality 6%), continues stirring to dodecyl sodium sulfonate
After sodium is completely dissolved, the reaction was continued 30 hours, stops stirring and heating, obtains monocycle oxygen terminated polysiloxane modified gelatin solution
(solution D).
The ratio of solution A, solution B, solution C and solution D 1:1:1:1 in mass ratio are mixed, gained viscosity of sludge is 790
Centipoise (50 DEG C) is added ethyl alcohol and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure baking oven
Drying 6 hours, obtains gelatin film,T gFor 195 DEG C and 200 DEG C, the contact angle of raw material gelatin film is 72 °, the gas/liquid face of Modified Membrane
Contact angle is 86 ° ± 2, solid-liquid face contact angle is 82 ° ± 2.
Embodiment 2:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:2:2:
1。
Gained viscosity of sludge is 760 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains modified gelatin film,T gFor 180 DEG C and 185 DEG C, gas/liquid face contact
Angle is 100 ° ± 2, and solid-liquid face contact angle is 98 ° ± 2.
Embodiment 3:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:3:1:
1。
Gained viscosity of sludge is 730 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 187 DEG C, gas/liquid face contact angle is
97 ° ± 2, solid-liquid face contact angle is 93 ° ± 2.
Embodiment 4:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:3:2:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 190 DEG C, gas/liquid face contact angle is
97 ° ± 2, solid-liquid face contact angle is 103 ° ± 2.
Embodiment 5:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:3:3:
1。
Gained viscosity of sludge is 745 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 195 DEG C and 165 DEG C, gas/liquid face contact angle is
85 ° ± 2, solid-liquid face contact angle is 122 ° ± 2, it is clear that has formed that gas/liquid face is hydrophilic, the strong hydrophobic parents' film in solid-liquid face.
Embodiment 6:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:4:1:
1。
Gained viscosity of sludge is 720 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 195 DEG C, gas/liquid face contact angle is
96 ° ± 2, solid-liquid face contact angle is 88 ° ± 2, and gas/liquid face shows as hydrophobic, and solid-liquid face shows as hydrophilic.
Embodiment 7:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:4:2:
1。
Gained viscosity of sludge is 725 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 182 DEG C, gas/liquid face contact angle is
102 ° ± 2, solid-liquid face contact angle is 100 ° ± 2.
Embodiment 8:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:4:3:
1。
Gained viscosity of sludge is 730 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 170 DEG C and 195 DEG C, gas/liquid face contact angle is
113 ° ± 2, solid-liquid face contact angle is 89 ° ± 2, and gas/liquid face shows as hydrophobic, and solid-liquid face shows as hydrophilic.
Embodiment 9:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 1:4:4:
1。
Gained viscosity of sludge is 735 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 170 DEG C and 185 DEG C, gas/liquid face contact angle is
115 ° ± 2, solid-liquid face contact angle is 96 ° ± 2.
Embodiment 10:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:1:2:
1.Gained viscosity of sludge is 755 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed
In normal pressure drying in oven 6 hours of 40 DEG C, gelatin film is obtained,T gFor 188 DEG C and 188 DEG C, gas/liquid face contact angle is 93 ° ±
2, solid-liquid face contact angle is 93 ° ± 2.
Embodiment 11:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:2:2:
1。
Gained viscosity of sludge is 750 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 185 DEG C, gas/liquid face contact angle is
102 ° ± 2, solid-liquid face contact angle is 96 ° ± 2.
Embodiment 12:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:3:2:
1。
Gained viscosity of sludge is 750 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 188 DEG C, gas/liquid face contact angle is
109 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 13:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:3:3:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 182 DEG C and 188 DEG C, gas/liquid face contact angle is
104 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 14:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:4:1:
1。
Gained viscosity of sludge is 760 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 188 DEG C, gas/liquid face contact angle is
95 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 15:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:4:2:
1。
Gained viscosity of sludge is 765 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 185 DEG C, gas/liquid face contact angle is
97 ° ± 2, solid-liquid face contact angle is 93 ° ± 2.
Embodiment 16:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:4:3:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 195 DEG C, gas/liquid face contact angle is
101 ° ± 2, solid-liquid face contact angle is 87 ° ± 2, and gas/liquid face shows as hydrophobicity, and solid-liquid face shows as hydrophily.
Embodiment 17:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:4:4:
1。
Gained viscosity of sludge is 810 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 200 DEG C and 180 DEG C, gas/liquid face contact angle is
83 ° ± 2, solid-liquid face contact angle is 100 ° ± 2, and the hydrophobicity of modified gelatin film improves.
Embodiment 18:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:5:1:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 200 DEG C, gas/liquid face contact angle is
102 ° ± 2, solid-liquid face contact angle is 82 ° ± 2, and gas/liquid face shows as hydrophobicity, and solid-liquid face shows as hydrophily.
Embodiment 19:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:5:2:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 200 DEG C, gas/liquid face contact angle is
107 ° ± 2, solid-liquid face contact angle is 83 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 20:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:5:3:
1。
Gained viscosity of sludge is 805 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is
108 ° ± 2, solid-liquid face contact angle is 88 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 21:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 2:5:4:
1。
Gained viscosity of sludge is 815 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 172 DEG C and 188 DEG C, gas/liquid face contact angle is
110 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 22:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:1:1:
1。
Gained viscosity of sludge is 720 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is
108 ° ± 2, solid-liquid face contact angle is 88 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 23:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:1:2:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 210 DEG C and 195 DEG C, gas/liquid face contact angle is
78 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 24:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:1:3:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 190 DEG C and 195 DEG C, gas/liquid face contact angle is
92 ° ± 2, solid-liquid face contact angle is 88 ° ± 2.
Embodiment 25:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:2:1:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 190 DEG C and 200 DEG C, gas/liquid face contact angle is
92 ° ± 2, solid-liquid face contact angle is 83 ° ± 2.
Embodiment 26:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:2:2:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 198 DEG C, gas/liquid face contact angle is
97 ° ± 2, solid-liquid face contact angle is 84 ° ± 2.
Embodiment 27:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:2:3:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 205 DEG C, gas/liquid face contact angle is
102 ° ± 2, solid-liquid face contact angle is 81 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 28:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:3:1:
1。
Gained viscosity of sludge is 755 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 178 DEG C and 200 DEG C, gas/liquid face contact angle is
105 ° ± 2, solid-liquid face contact angle is 85 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 29:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:3:2:
1。
Gained viscosity of sludge is 795 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is
106 ° ± 2, solid-liquid face contact angle is 87 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 30:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:3:3:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 185 DEG C, gas/liquid face contact angle is
107 ° ± 2, solid-liquid face contact angle is 96 ° ± 2.
Embodiment 31:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:5:1:
1。
Gained viscosity of sludge is 780 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 180 DEG C, gas/liquid face contact angle is
103 ° ± 2, solid-liquid face contact angle is 100 ° ± 2.
Embodiment 32:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:5:2:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 185 DEG C, gas/liquid face contact angle is
108 ° ± 2, solid-liquid face contact angle is 96 ° ± 2.
Embodiment 33:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:5:3:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 185 DEG C, gas/liquid face contact angle is
108 ° ± 2, solid-liquid face contact angle is 96 ° ± 2.
Embodiment 34:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:5:4:
1。
Gained viscosity of sludge is 810 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 186 DEG C, gas/liquid face contact angle is
100 ° ± 2, solid-liquid face contact angle is 96 ° ± 2.
Embodiment 35:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 3:5:5:
1。
Gained viscosity of sludge is 820 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 182 DEG C, gas/liquid face contact angle is
109 ° ± 2, solid-liquid face contact angle is 93 ° ± 2.
Embodiment 36:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:1:1:
1。
Gained viscosity of sludge is 710 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 200 DEG C, gas/liquid face contact angle is
95 ° ± 2, solid-liquid face contact angle is 82 ° ± 2.
Embodiment 37:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:1:2:
1。
Gained viscosity of sludge is 730 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 220 DEG C and 240 DEG C, gas/liquid face contact angle is
69 ° ± 2, solid-liquid face water imbibition is very strong.
Embodiment 38:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:1:3:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 210 DEG C, gas/liquid face contact angle is
104 ° ± 2, solid-liquid face contact angle is 78 ° ± 2.
Embodiment 39:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:1:4:
1。
Gained viscosity of sludge is 750 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is
108 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 40:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:2:1:
1。
Gained viscosity of sludge is 725 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 195 DEG C, gas/liquid face contact angle is
100 ° ± 2, solid-liquid face contact angle is 87 ° ± 2, gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 41:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:2:2:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 188 DEG C and 205 DEG C, gas/liquid face contact angle is
93 ° ± 2, solid-liquid face contact angle is 80 ° ± 2.
Embodiment 42:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:2:3:
1。
Gained viscosity of sludge is 760 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 178 DEG C, gas/liquid face contact angle is
101 ° ± 2, solid-liquid face contact angle is 106 ° ± 2.
Embodiment 43:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:2:4:
1。
Gained viscosity of sludge is 780 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 160 DEG C and 195 DEG C, gas/liquid face contact angle is
119 ° ± 2, solid-liquid face contact angle is 86 ° ± 2, gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 44:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:3:4:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 180 DEG C, gas/liquid face contact angle is
100 ° ± 2, solid-liquid face contact angle is 100 ° ± 2.
Embodiment 45:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:4:4:
1。
Gained viscosity of sludge is 810 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 195 DEG C and 200 DEG C, gas/liquid face contact angle is
90 ° ± 2, solid-liquid face contact angle is 87 ° ± 2.
Embodiment 46:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:5:1:
1。
Gained viscosity of sludge is 780 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 180 DEG C, gas/liquid face contact angle is
111 ° ± 2, solid-liquid face contact angle is 104 ° ± 2.
Embodiment 47:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:5:2:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 165 DEG C and 240 DEG C, gas/liquid face contact angle is
116 ° ± 2, solid-liquid face contact angle is 20 ° ± 2, relatively strong hydrophobic, the solid-liquid face strong hydrophilicity in gas/liquid face.
Embodiment 48:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:5:3:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 165 DEG C and 185 DEG C, gas/liquid face contact angle is
115 ° ± 2, solid-liquid face contact angle is 98 ° ± 2.
Embodiment 49:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:5:4:
1。
Gained viscosity of sludge is 810 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 178 DEG C and 185 DEG C, gas/liquid face contact angle is
105 ° ± 2, solid-liquid face contact angle is 97 ° ± 2.
Embodiment 50:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 4:5:5:
1。
Gained viscosity of sludge is 830 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 160 DEG C and 200 DEG C, gas/liquid face contact angle is
119 ° ± 2, solid-liquid face contact angle is 83 ° ± 2, and gas/liquid face is hydrophobic by force, and solid-liquid face is hydrophilic.The section elemental analysis of gelatin film
In, Si element is assembled in gas/liquid face, and solid-liquid face is practically free of Si element (see Figure of description).
Embodiment 51:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:1:1:
1。
Gained viscosity of sludge is 715 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 172 DEG C and 180 DEG C, gas/liquid face contact angle is
111 ° ± 2, solid-liquid face contact angle is 99 ° ± 2.
Embodiment 52:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:1:2:
1。
Gained viscosity of sludge is 730 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 145 DEG C and 180 DEG C, gas/liquid face contact angle is
131 ° ± 2, solid-liquid face contact angle is 99 ° ± 2, and gas/liquid face is hydrophobic by force.
Embodiment 53:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:1:3:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 180 DEG C, gas/liquid face contact angle is
102 ° ± 2, solid-liquid face contact angle is 101 ° ± 2.
Embodiment 54:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:1:4:
1。
Gained viscosity of sludge is 755 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 180 DEG C, gas/liquid face contact angle is
107 ° ± 2, solid-liquid face contact angle is 103 ° ± 2.
Embodiment 55:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:1:5:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 180 DEG C, gas/liquid face contact angle is
96 ° ± 2, solid-liquid face contact angle is 101 ° ± 2.
Embodiment 56:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:2:1:
1。
Gained viscosity of sludge is 720 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 180 DEG C, gas/liquid face contact angle is
101 ° ± 2, solid-liquid face contact angle is 101 ° ± 2.
Embodiment 57:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:2:2:
1。
Gained viscosity of sludge is 730 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 179 DEG C, gas/liquid face contact angle is
110 ° ± 2, solid-liquid face contact angle is 106 ° ± 2.
Embodiment 58:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:2:3:
1。
Gained viscosity of sludge is 745 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 172 DEG C and 188 DEG C, gas/liquid face contact angle is
112 ° ± 2, solid-liquid face contact angle is 94 ° ± 2.
Embodiment 59:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:2:4:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 178 DEG C and 185 DEG C, gas/liquid face contact angle is
105 ° ± 2, solid-liquid face contact angle is 97 ° ± 2.
Embodiment 60:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:2:5:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 190 DEG C, gas/liquid face contact angle is
107 ° ± 2, solid-liquid face contact angle is 92 ° ± 2.
Embodiment 61:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:3:1:
1。
Gained viscosity of sludge is 740 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 173 DEG C and 175 DEG C, gas/liquid face contact angle is
111 ° ± 2, solid-liquid face contact angle is 110 ° ± 2.
Embodiment 62:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:3:2:
1。
Gained viscosity of sludge is 760 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 182 DEG C and 160 DEG C, gas/liquid face contact angle is
100 ° ± 2, solid-liquid face contact angle is 118 ° ± 2.
Embodiment 63:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:3:3:
1。
Gained viscosity of sludge is 780 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is
110 ° ± 2, solid-liquid face contact angle is 86 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 64:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:3:4:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 180 DEG C, gas/liquid face contact angle is
110 ° ± 2, solid-liquid face contact angle is 102 ° ± 2.
Embodiment 65:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:3:5:
1。
Gained viscosity of sludge is 800 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 168 DEG C and 195 DEG C, gas/liquid face contact angle is
115 ° ± 2, solid-liquid face contact angle is 90 ° ± 2.
Embodiment 66:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:4:1:
1。
Gained viscosity of sludge is 750 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 165 DEG C and 182 DEG C, gas/liquid face contact angle is
116 ° ± 2, solid-liquid face contact angle is 99 ° ± 2.
Embodiment 67:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:4:2:
1。
Gained viscosity of sludge is 760 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 169 DEG C and 180 DEG C, gas/liquid face contact angle is
114 ° ± 2, solid-liquid face contact angle is 101 ° ± 2.
Embodiment 68:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:4:3:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 170 DEG C and 178 DEG C, gas/liquid face contact angle is
113 ° ± 2, solid-liquid face contact angle is 107 ° ± 2.
Embodiment 69:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:4:4:
1。
Gained viscosity of sludge is 780 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 185 DEG C and 205 DEG C, gas/liquid face contact angle is
96 ° ± 2, solid-liquid face contact angle is 80 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 70:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:4:5:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 178 DEG C, gas/liquid face contact angle is
109 ° ± 2, solid-liquid face contact angle is 107 ° ± 2.
Embodiment 71:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:5:1:
1。
Gained viscosity of sludge is 750 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 155 DEG C and 178 DEG C, gas/liquid face contact angle is
123 ° ± 2, solid-liquid face contact angle is 105 ° ± 2.
Embodiment 72:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:5:2:
1。
Gained viscosity of sludge is 760 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 195 DEG C and 178 DEG C, gas/liquid face contact angle is
89 ° ± 2, solid-liquid face contact angle is 105 ° ± 2.
Embodiment 73:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:5:3:
1。
Gained viscosity of sludge is 770 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 198 DEG C, gas/liquid face contact angle is
107 ° ± 2, solid-liquid face contact angle is 86 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 74:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:5:4:
1。
Gained viscosity of sludge is 780 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 183 DEG C and 182 DEG C, gas/liquid face contact angle is
99 ° ± 2, solid-liquid face contact angle is 100 ° ± 2.
Embodiment 75:
Described method and embodiment 1 are consistent, are not uniquely both that solution A, the proportion of B, C, D are changed to mass ratio 5:5:5:
1。
Gained viscosity of sludge is 790 centipoises (50 DEG C), and ethyl alcohol is added and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:
4, it is placed in 40 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 180 DEG C, gas/liquid face contact angle is
108 ° ± 2, solid-liquid face contact angle is 101 ° ± 2.
Embodiment 76:
Described method and embodiment 50 are consistent, and solution temperature is substituted for 40 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 195 DEG C and 223 DEG C, gas/liquid face contact angle is 89 ° ± 2, solid-liquid face contact angle is 210 ° ±
2, it is two-sided all hydrophilic.
Embodiment 77:
Described method and embodiment 50 are consistent, and solution temperature is substituted for 60 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 185 DEG C and 205 DEG C, gas/liquid face contact angle is 95 ° ± 2, solid-liquid face contact angle is 80 ° ±
2。
Embodiment 78:
Described method and embodiment 50 are consistent, are not uniquely both that pH is substituted for 8.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 205 DEG C and 215 DEG C, gas/liquid face contact angle is 78 ° ± 2, solid-liquid face contact angle is 72 ° ±
2, it is two-sided all hydrophilic.
Embodiment 79:
Described method and embodiment 50 are consistent, are not uniquely both that pH is substituted for 9.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 196 DEG C and 195 DEG C, gas/liquid face contact angle is 91 ° ± 2, solid-liquid face contact angle is 89 ° ±
2。
Embodiment 80:
Described method and embodiment 50 are consistent, are not uniquely both that pH is substituted for 11.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 195 DEG C and 198 DEG C, gas/liquid face contact angle is 87 ° ± 2, solid-liquid face contact angle is 83 ° ±
2。
Embodiment 81:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 0.04:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 220 DEG C and 225 DEG C, gas/liquid face contact angle is 69 ° ± 2, solid-liquid face contact angle is 65 ° ±
2。
Embodiment 82:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 0.1:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 215 DEG C and 217 DEG C, gas/liquid face contact angle is 72 ° ± 2, solid-liquid face contact angle is 70 ° ±
2, it is two-sided all hydrophilic.
Embodiment 83:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 0.5:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 195 DEG C and 215 DEG C, gas/liquid face contact angle is 90 ° ± 2, solid-liquid face contact angle is 73 ° ±
2。
Embodiment 84:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 1:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is 110 ° ± 2, solid-liquid face contact angle is 89 ° ±
2。
Embodiment 85:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 1.5:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 198 DEG C and 205 DEG C, gas/liquid face contact angle is 83 ° ± 2, solid-liquid face contact angle is 79 ° ±
2。
Embodiment 86:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 2:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 215 DEG C and 217 DEG C, gas/liquid face contact angle is 73 ° ± 2, solid-liquid face contact angle is 70 ° ±
2, it is two-sided all hydrophilic.
Embodiment 87:
Described method and embodiment 50 are consistent, are not uniquely both that the molar ratio of monocycle oxygen terminated polysiloxane and gelatin is replaced
Change 3:1 into.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 40 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 217 DEG C and 220 DEG C, gas/liquid face contact angle is 70 ° ± 2, solid-liquid face contact angle is 68 ° ±
2, it is two-sided all hydrophilic.
Embodiment 88:
Described method and embodiment 50 are consistent, are not uniquely both that drying temperature is substituted for 25 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 50 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 183 DEG C and 195 DEG C, gas/liquid face contact angle is 93 ° ± 2, solid-liquid face contact angle is 89 ° ±
2。
Embodiment 89:
Described method and embodiment 50 are consistent, are not uniquely both that drying temperature is substituted for 35 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 50 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 185 DEG C and 210 DEG C, gas/liquid face contact angle is 96 ° ± 2, solid-liquid face contact angle is 77 ° ±
2。
Embodiment 90:
Described method and embodiment 50 are consistent, are not uniquely both that drying temperature is substituted for 50 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 60 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 170 DEG C and 195 DEG C, gas/liquid face contact angle is 105 ° ± 2, solid-liquid face contact angle is 90 ° ±
2。
Embodiment 91:
Described method and embodiment 50 are consistent, are not uniquely both that drying temperature is substituted for 60 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 60 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 175 DEG C and 195 DEG C, gas/liquid face contact angle is 108 ° ± 2, solid-liquid face contact angle is 89 ° ±
2。
Embodiment 92:
Described method and embodiment 50 are consistent, are not uniquely both that drying temperature is substituted for 70 DEG C.
Ethyl alcohol is added to be uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, is placed in 60 DEG C of normal pressure drying in oven
6 hours, gelatin film is obtained,T gFor 175 DEG C and 185 DEG C, gas/liquid face contact angle is 108 ° ± 2, solid-liquid face contact angle is 95 ° ±
2。
Embodiment 93:
Described method and embodiment 50 are consistent, are not uniquely both to insert equipped with thermometer socket, sample tap and condenser
3 grams of gelatin (account for gross mass 3%), 97 grams of deionized waters are added in three mouthfuls of reaction flasks of mouth, gained viscosity of sludge is 400 centipoises
(50 DEG C) are added ethyl alcohol and are uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:4, are placed in 60 DEG C of normal pressure drying in oven 6
Hour, gelatin film is obtained,T gFor 185 DEG C and 205 DEG C, gas/liquid face contact angle is 96 ° ± 2, and solid-liquid face contact angle is 80 ° ± 2.
Embodiment 94:
Described method and embodiment 1 are consistent, are not uniquely both equipped with thermometer socket, sample tap and condenser socket
Three mouthfuls of reaction flasks in be added 8 grams of gelatin (account for gross mass 8%), 92 grams of deionized waters, gained viscosity of sludge be 950 centipoises (50
DEG C), ethyl alcohol is added and is uniformly mixed, the volume ratio of ethyl alcohol and mixed liquor is 1:4, and it is small to be placed in 60 DEG C of normal pressure drying in oven 6
When, gelatin film is obtained,T gFor 183 DEG C and 195 DEG C, gas/liquid face contact angle is 93 ° ± 2, and solid-liquid face contact angle is 89 ° ± 2.
Embodiment 95:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:1.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 198 DEG C and 205 DEG C, gas/liquid face is connect
Feeler is 85 ° ± 2, and solid-liquid face contact angle is 79 ° ± 2.
Embodiment 96:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:2.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 183 DEG C and 195 DEG C, gas/liquid face is connect
Feeler is 93 ° ± 2, and solid-liquid face contact angle is 89 ° ± 2.
Embodiment 97:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:3.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 175 DEG C and 198 DEG C, gas/liquid face is connect
Feeler is 107 ° ± 2, and solid-liquid face contact angle is 86 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 98:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:5.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 178 DEG C and 195 DEG C, gas/liquid face is connect
Feeler is 105 ° ± 2, and solid-liquid face contact angle is 90 ° ± 2.
Embodiment 99:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:6.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 180 DEG C and 195 DEG C, gas/liquid face is connect
Feeler is 100 ° ± 2, and solid-liquid face contact angle is 86 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 100:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:7.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,gFor 185 DEG C and 200 DEG C, gas/liquid face is connect
Feeler is 95 ° ± 2, and solid-liquid face contact angle is 82 ° ± 2, and gas/liquid face is hydrophobic, and solid-liquid face is hydrophilic.
Embodiment 101:
Described method and embodiment 50 are consistent, are not uniquely both that the volume ratio of ethyl alcohol and mixed liquor replaces with 1:8.
It is placed in 60 DEG C of normal pressure drying in oven 6 hours, obtains gelatin film,T gFor 195 DEG C and 205 DEG C, gas/liquid face is connect
Feeler is 87 ° ± 2, and solid-liquid face contact angle is 79 ° ± 2.
Claims (3)
1. a kind of preparation method of monocycle oxygen terminated polysiloxane modified gelatin parents' film, which comprises the steps of:
(1) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 500, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution A);
(2) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 1000, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution B);
(3) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 2000, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution C);
(4) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
Be 10.0, be added 0.3g sodium alkyl sulfonate, continue stirring be completely dissolved to dodecyl sodium sulfate after, the reaction was continued 30 hours,
Stop stirring and heating, obtains solution D;
(5) ratio of solution A, solution B, solution C and solution D 1:3:3:1 in mass ratio are mixed, gained viscosity of sludge is 745
Centipoise is added ethyl alcohol and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:4, and it is small to be placed in 40 DEG C of normal pressure drying in oven 6
When, obtain gelatin film.
2. a kind of preparation method of monocycle oxygen terminated polysiloxane modified gelatin parents' film, which comprises the steps of:
(1) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 500, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution A);
(2) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 1000, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution B);
(3) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 2000, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution C);
(4) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
Be 10.0, be added 0.3g sodium alkyl sulfonate, continue stirring be completely dissolved to dodecyl sodium sulfate after, the reaction was continued 30 hours,
Stop stirring and heating, obtains solution D;
(5) ratio of solution A, solution B, solution C and solution D 4:5:5:1 in mass ratio are mixed, gained viscosity of sludge is 830
Centipoise is added ethyl alcohol and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:4, and it is small to be placed in 40 DEG C of normal pressure drying in oven 6
When, obtain gelatin film.
3. a kind of preparation method of monocycle oxygen terminated polysiloxane modified gelatin parents' film, which comprises the steps of:
(1) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 500, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution A);
(2) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 1000, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution B);
(3) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
It is 10.0,0.3g sodium alkyl sulfonate is added, continues after stirring is completely dissolved to dodecyl sodium sulfate, it is continuous or be added portionwise point
The molar ratio of the monocycle oxygen terminated polysiloxane that son amount is 2000, monocycle oxygen terminated polysiloxane and gelatin is 0.8:1, and reaction is opened
Begin, the content of primary amine group reacted in 24 hours systems is no longer changed, and stops stirring and heating, obtains single epoxy-capped poly- silicon
Siloxane modified gelatin solution (solution C);
(4) equipped with thermometer socket, sample tap and condenser socket three mouthfuls of reaction flasks in be added 5 grams of gelatin, 95 grams go from
Sub- water is heated with stirring to 50 DEG C, and after gelatin is completely dissolved, the sodium hydroxide of 0.65mL2 mol/L is added, and adjusts reaction pH
Be 10.0, be added 0.3g sodium alkyl sulfonate, continue stirring be completely dissolved to dodecyl sodium sulfate after, the reaction was continued 30 hours,
Stop stirring and heating, obtains solution D;
(5) ratio of solution A, solution B, solution C and solution D 4:5:5:1 in mass ratio are mixed, gained viscosity of sludge is 830
Centipoise is added ethyl alcohol and is uniformly mixed, and the volume ratio of ethyl alcohol and mixed liquor is 1:3, and it is small to be placed in 60 DEG C of normal pressure drying in oven 6
When, obtain gelatin film.
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