CN109206818A - A kind of preparation method of the evenly dispersed type hydrogel of high intensity - Google Patents
A kind of preparation method of the evenly dispersed type hydrogel of high intensity Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of the evenly dispersed type hydrogel of high intensity, belong to hydrogel preparation technical field.The present invention obtains oxidation mixed liquor as raw material using bamboo plate and reacts with hydrogen peroxide, soybean lecithin is added and is mixed to prepare mixed serum, mixed serum is digested again, reaction lotion is made after concentration, lotion and acrylamide will finally be reacted, distilled water and other auxiliary agents are mixed to prepare high-intensitive evenly dispersed type hydrogel, bamboo fibre and graphite powder hybrid reaction are generated graphene oxide by the present invention, in sulfuric acid solution, graphene oxide is promoted to be come into full contact with bamboo fibre, being conducive to hydrogel, crosslink density is improved after hardening, the present invention is using bamboo fibre as substrate, graphene oxide is attached in bamboo fibre pipe, and bamboo fibre is mixed with soybean lecithin, effectively strengthen the mechanical property after water-setting adhesive curing, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of the evenly dispersed type hydrogel of high intensity, belong to hydrogel technology of preparing neck
Domain.
Background technique
Gel is seen everywhere in our daily lifes usually, such as jelly, agar, toothpaste, contact lenses, glue-type steel
Pen, hair jelly and other cosmetics etc., wherein hydrogel is most commonly seen.Hydrogel is by hydrophilic macromolecular chain by being crosslinked
The tridimensional network material of formation, since it swells in water, soft and similar biological tissue, is a kind of ideal life
Object compatibility material.Hydrogel is a kind of functional polymer material quickly grown, in biological medicine, enzymatic activity control, molecule
The fields such as separation have a wide range of applications.
The research of hydrogel has driven the development of related discipline such as medicine, biotechnology, water and soil, material science etc..
However when hydrogel is used for these fields, it is usually required with certain intensity, to meet as load or keep it
Functional requirement.And traditional synthesizing high-hydroscopicity gel is mainly using acrylic acid, acrylamide as raw material, the water of homogenous material
Since crosslink density is low and cross-linked structure is uneven, gel stretches low with compressive strength etc. insufficient gel after water suction, serious to limit
Its development is made.Further, since containing a large amount of water inside hydrogel, viscosity is extremely limited.However, at present mostly
Several research work focuses primarily upon the mechanical property for improving hydrogel, and extremely limited to the research of its viscosity.Hydrogel
Excellent adhering performance depends on the equilibrium relation of aquogel system good cohesive force and cohesive force.Wherein, when hydrogel
When cohesive force is larger, polymer generates effective cementation with stromal surface and will be restricted, and works as the bonding of hydrogel
When power is larger, the weaker mechanical property for leading to hydrogel is low again for cohesive force, is unable to satisfy hydrogel answering under a large load
With which limits the application ranges of hydrogel.
Therefore, it develops while there is the hydrogel of excellent viscosity and mechanical strength appropriate to be particularly important.
Summary of the invention
The technical problems to be solved by the invention: cause hydrogel easy for mechanical property is bad after the solidification of current hydrogel
Fracture, while it being directed to the non-uniform defect of hydrogel internal structure, provide a kind of system of evenly dispersed type hydrogel of high intensity
Preparation Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of the evenly dispersed type hydrogel of high intensity, it is characterised in that specific preparation step are as follows:
(1) it weighs in 500~700g bamboo plate investment beaker, impregnates bamboo plate with sodium hydroxide solution, place the beaker water-bath
In pot, mixed liquor is made in 3~5h of constant temperature boiling, and graphite powder is added in beaker, is mixed with blender, filter is obtained by filtration
Slag, wash with distilled water filter residue 3~5 times；
(2) by after the grinding of above-mentioned filter residue and in sulfuric acid solution 1:5 in mass ratio investment three-necked flask, it is mixed that solid-liquid is made in sonic oscillation
Object is closed, the potassium permanganate powder of solidliquid mixture quality 5~8% is added into three-necked flask, is mixed with blender and oxygen is made
Change mixed liquor；
(3) hydrogen peroxide of oxidation mixed liquor quality 40~60% is added into above-mentioned three-necked flask, places the beaker permanent in water-bath
Temperature reaction, is obtained by filtration filter cake after reaction, will mix in filter cake and soybean lecithin aqueous solution 1:5 in mass ratio investment reaction kettle
Even obtained mixed serum；
(4) by mixed serum and cellulase 60:1 in mass ratio investment glass dish, glass dish is placed in climatic chamber,
Under argon atmosphere, mixed emulsion is made in 4~6h of sealing and standing, and the soybean of mixed emulsion quality 8~12% is added into glass dish
Albumen powder continues 2~3h of sealing and standing under argon atmosphere after mixing, glass dish is placed in microwave reactor after standing
Microwave treatment, then glass dish is placed in a vacuum drying oven vacuum concentration, reaction lotion is made；
(5) score meter by weight, weighs 7~9 parts of above-mentioned reaction lotions, 1~2 part of potassium peroxydisulfate, 8~10 parts of acrylamides and 20
In~22 parts of deionized water investment beakers, places the beaker in water-bath, be mixed with blender, cooled to room temperature is
Obtain high-intensitive evenly dispersed type hydrogel.
The mass fraction of sodium hydroxide solution as described in step (1) is 10~15%, the bath temperature of water-bath is 95~
100 DEG C, the constant temperature boiling time is 3~5h, and the revolving speed of blender is 400~500r/min, and mixing time is 3~4h.
The mass fraction of sulfuric acid solution described in step (2) is 40~50%, and supersonic frequency is 30~32kHz, water-bath temperature
Degree is 5~10 DEG C, and duration of oscillation is 3~4h, and the revolving speed of blender is 500~600r/min, and mixing time is 3~4h.
The mass fraction of hydrogen peroxide described in step (3) is 20~25%, and the bath temperature in water-bath is 30~35
DEG C, the isothermal reaction time is 30~40min, and the mass fraction of soybean lecithin aqueous solution is 20~25%.
The sealing and standing time is 4~6h in climatic chamber described in step (4), and the power of microwave reactor is 700
~800W, microwave treatment time are 10~15min, and the temperature of vacuum oven is 30~35 DEG C, and vacuum degree is 50~80Pa, very
Empty concentration time is 100~120min.
Bath temperature in water-bath described in step (5) is 50~60 DEG C, the revolving speed of blender is 1000~
1100r/min, mixing time are 40~50min.
The method have the benefit that:
(1) graphite powder mixing oscillation, filtering are added first by bamboo plate and sodium hydroxide solution hybrid reaction, after reaction by the present invention
Filter residue is obtained, filter residue is mixed with sulfuric acid, potassium permanganate reaction is added after mixing, oxidation mixed liquor is made, then mix oxidation
Liquid is reacted with hydrogen peroxide, and soybean lecithin is added after reaction and is mixed to prepare mixed serum, then mixed serum is digested, after enzymatic hydrolysis
Soybean protein is added and carries out enzyme digestion reaction again, reaction lotion is made after concentration, it finally will reaction lotion and acrylamide, distillation
Water and other auxiliary agents are mixed to prepare high-intensitive evenly dispersed type hydrogel, and the present invention, which mixes bamboo fibre with graphite powder, carries out oxygen
Change reaction, graphite powder reaction is made to generate graphene oxide, makes to introduce in bamboo fibre surface and graphene molecules under sulfuric acid immersion
Sulfonic acid group has the functional groups such as sulfonic group, hydroxyl, carboxyl in graphene oxide, under the conditions of existing for the bamboo fibre, absorption knot
Together on bamboo fibre, while in sulfuric acid solution, the removing dispersion between bamboo fibre is more complete, promotes graphene oxide and bamboo
Fiber is come into full contact with, and bamboo fibre passes through each functional group having in itself and graphene oxide to other in hydrogel
Molecule forms covalent bond, hydrogen bond and the absorption of other Chemical bondings, and being conducive to hydrogel, crosslink density is mentioned after hardening
Height is difficult to be broken to reinforce the mechanical property after water-setting adhesive curing after making water-setting adhesive curing；
(2) graphene oxide is attached in bamboo fibre pipe by the present invention using bamboo fibre as substrate, and by bamboo fibre and soybean lecithin
Mixing makes soybean lecithin and bamboo fibre is evenly dispersed dissolves each other by cellulase hydrolysis, make in soybean lecithin each phospholipid composition with
And other organic components adsorbed closes are on bamboo fibre pipe, and are crosslinked mutually with graphene oxide therein, not only make bamboo fine
Tie up it is eased be scattered in hydrogel, the mechanical property after more effectively strengthening water-setting adhesive curing, after making water-setting adhesive curing
Tearing-resistant performance and Adhesion property further reinforced, have broad application prospects.
Specific embodiment
It weighs in 500~700g bamboo plate investment beaker, impregnates hair with the sodium hydroxide solution that mass fraction is 10~15%
Bamboo chip places the beaker in the water-bath that bath temperature is 95~100 DEG C, and mixed liquor is made in 3~5h of constant temperature boiling, by graphite powder
It is added in beaker, 3~4h is mixed with the revolving speed of 400~500r/min with blender, filter residue is obtained by filtration, it is clear with distilled water
Filter wash slag 3~5 times；By three mouthfuls of sulfuric acid solution 1:5 in mass ratio investment for being 40~50% with mass fraction after the grinding of above-mentioned filter residue
In flask, 3~4h is vibrated under conditions of supersonic frequency is 30~32kHz and bath temperature is 5~10 DEG C, and solid-liquid mixing is made
Object the potassium permanganate powder of solidliquid mixture quality 5~8% is added into three-necked flask, with blender with 500~600r/min
Revolving speed be mixed 3~4h, be made oxidation mixed liquor；Oxidation mixed liquor quality 40~60% is added into above-mentioned three-necked flask
Mass fraction be 20~25% hydrogen peroxide, placing the beaker bath temperature is isothermal reaction 30 in 30~35 DEG C of water-bath
Filter cake is obtained by filtration after reaction in~40min, by filter cake and mass fraction be 20~25% soybean lecithin aqueous solution in mass ratio
1:5, which is put into reaction kettle, is uniformly mixed obtained mixed serum；Mixed serum and cellulase 60:1 in mass ratio are put into glass
In ware, glass dish is placed in climatic chamber, under argon atmosphere, mixed emulsion is made in 4~6h of sealing and standing, to glass dish
The middle soyabean protein powder that mixed emulsion quality 8~12% is added, continues 2~3h of sealing and standing under argon atmosphere after mixing,
Glass dish is placed in microwave reactor after standing, 10~15min of microwave treatment under conditions of power is 700~800W, then
Glass dish is placed in a vacuum drying oven, is concentrated in vacuo 100 under conditions of temperature is 30~35 DEG C, vacuum degree is 50~80Pa
Reaction lotion is made in~120min；Score meter by weight weighs 7~9 parts of above-mentioned reaction lotions, 1~2 part of potassium peroxydisulfate, 8~10
In part acrylamide and 20~22 parts of deionized waters investment beakers, the water-bath that bath temperature is 50~60 DEG C is placed the beaker
In, 40~50min is mixed with the revolving speed of 1000~1100r/min with blender, cooled to room temperature is up to high-intensitive
Evenly dispersed type hydrogel.
It weighs in 500g bamboo plate investment beaker, impregnates bamboo plate with the sodium hydroxide solution that mass fraction is 10%, will burn
Cup is placed in the water-bath that bath temperature is 95 DEG C, and mixed liquor is made in constant temperature boiling 3h, graphite powder is added in beaker, with stirring
3h is mixed with the revolving speed of 400r/min in device, filter residue is obtained by filtration, wash with distilled water filter residue 3 times；Above-mentioned filter residue is ground
The sulfuric acid solution 1:5 in mass ratio for being afterwards 40% with mass fraction is put into three-necked flask, is 30kHz and water-bath in supersonic frequency
Temperature vibrates 3h under conditions of being 5 DEG C, and solidliquid mixture is made, and the Gao Meng of solidliquid mixture quality 5% is added into three-necked flask
Sour potassium powder is mixed 3h with blender with the revolving speed of 500r/min, oxidation mixed liquor is made；Add into above-mentioned three-necked flask
Enter to aoxidize the hydrogen peroxide that the mass fraction of mixed liquor quality 40% is 20%, places the beaker the water-bath that bath temperature is 30 DEG C
In, filter cake is obtained by filtration after reaction in isothermal reaction 30min, and the soybean lecithin aqueous solution that filter cake and mass fraction are 20% is pressed matter
Amount is than being uniformly mixed obtained mixed serum in 1:5 investment reaction kettle；Mixed serum and cellulase 60:1 in mass ratio are put into
In glass dish, glass dish is placed in climatic chamber, under argon atmosphere, mixed emulsion is made in sealing and standing 4h, to glass
The soyabean protein powder of mixed emulsion quality 8% is added in ware, continues the sealing and standing 2h under argon atmosphere after mixing, stands
Glass dish is placed in microwave reactor afterwards, microwave treatment 10min under conditions of power is 700W, then glass dish is placed in very
In empty drying box, it is concentrated in vacuo 100min under conditions of temperature is 30 DEG C, vacuum degree is 50Pa, reaction lotion is made；By weight
Score meter weighs in 7 parts of above-mentioned reaction lotions, 1 part of potassium peroxydisulfate, 8 parts of acrylamides and 20 parts of deionized water investment beakers, will
Beaker is placed in the water-bath that bath temperature is 50 DEG C, and 40min is mixed with the revolving speed of 1000r/min with blender, natural
It is cooled to room temperature up to high-intensitive evenly dispersed type hydrogel.
It weighs in 600g bamboo plate investment beaker, impregnates bamboo plate with the sodium hydroxide solution that mass fraction is 13%, will burn
Cup is placed in the water-bath that bath temperature is 97 DEG C, and mixed liquor is made in constant temperature boiling 4h, graphite powder is added in beaker, with stirring
4h is mixed with the revolving speed of 450r/min in device, filter residue is obtained by filtration, wash with distilled water filter residue 4 times；Above-mentioned filter residue is ground
The sulfuric acid solution 1:5 in mass ratio for being afterwards 45% with mass fraction is put into three-necked flask, is 31kHz and water-bath in supersonic frequency
Temperature vibrates 3h under conditions of being 7 DEG C, and solidliquid mixture is made, and the Gao Meng of solidliquid mixture quality 7% is added into three-necked flask
Sour potassium powder is mixed 3h with blender with the revolving speed of 550r/min, oxidation mixed liquor is made；Add into above-mentioned three-necked flask
Enter to aoxidize the hydrogen peroxide that the mass fraction of mixed liquor quality 50% is 23%, places the beaker the water-bath that bath temperature is 33 DEG C
In, filter cake is obtained by filtration after reaction in isothermal reaction 35min, and the soybean lecithin aqueous solution that filter cake and mass fraction are 23% is pressed matter
Amount is than being uniformly mixed obtained mixed serum in 1:5 investment reaction kettle；Mixed serum and cellulase 60:1 in mass ratio are put into
In glass dish, glass dish is placed in climatic chamber, under argon atmosphere, mixed emulsion is made in sealing and standing 5h, to glass
The soyabean protein powder of mixed emulsion quality 10% is added in ware, continues the sealing and standing 2h under argon atmosphere after mixing, stands
Glass dish is placed in microwave reactor afterwards, microwave treatment 13min under conditions of power is 750W, then glass dish is placed in very
In empty drying box, it is concentrated in vacuo 110min under conditions of temperature is 33 DEG C, vacuum degree is 60Pa, reaction lotion is made；By weight
Score meter weighs in 8 parts of above-mentioned reaction lotions, 1 part of potassium peroxydisulfate, 9 parts of acrylamides and 21 parts of deionized water investment beakers, will
Beaker is placed in the water-bath that bath temperature is 55 DEG C, and 45min is mixed with the revolving speed of 1050r/min with blender, natural
It is cooled to room temperature up to high-intensitive evenly dispersed type hydrogel.
It weighs in 700g bamboo plate investment beaker, impregnates bamboo plate with the sodium hydroxide solution that mass fraction is 15%, will burn
It is in 100 DEG C of water-bath that cup, which is placed in bath temperature, and mixed liquor is made in constant temperature boiling 5h, by graphite powder addition beaker, with stirring
It mixes device and 4h is mixed with the revolving speed of 500r/min, filter residue is obtained by filtration, wash with distilled water filter residue 5 times；Above-mentioned filter residue is ground
The sulfuric acid solution 1:5 in mass ratio for being 50% with mass fraction after mill is put into three-necked flask, is 32kHz and water in supersonic frequency
Bath temperature vibrates 4h under conditions of being 10 DEG C, and solidliquid mixture is made, and solidliquid mixture quality 8% is added into three-necked flask
Potassium permanganate powder is mixed 4h with blender with the revolving speed of 600r/min, oxidation mixed liquor is made；To above-mentioned three-necked flask
The hydrogen peroxide that the middle mass fraction that oxidation mixed liquor quality 60% is added is 25%, places the beaker the water-bath that bath temperature is 35 DEG C
In pot, filter cake is obtained by filtration after reaction in isothermal reaction 40min, and the soybean lecithin aqueous solution that filter cake is 25% with mass fraction is pressed
Mass ratio 1:5, which is put into reaction kettle, is uniformly mixed obtained mixed serum；Mixed serum and cellulase 60:1 in mass ratio are thrown
Enter in glass dish, glass dish is placed in climatic chamber, under argon atmosphere, mixed emulsion is made in sealing and standing 6h, to glass
The soyabean protein powder of mixed emulsion quality 12% is added in glass ware, continues the sealing and standing 3h under argon atmosphere after mixing, it is quiet
It postpones and glass dish is placed in microwave reactor, microwave treatment 15min under conditions of power is 800W, then glass dish is placed in
In vacuum oven, it is concentrated in vacuo 120min under conditions of temperature is 35 DEG C, vacuum degree is 80Pa, reaction lotion is made；By weight
Score meter is measured, 9 parts of above-mentioned reaction lotions, 2 parts of potassium peroxydisulfates, 10 parts of acrylamides and 22 parts of deionized water investment beakers are weighed
In, it places the beaker in the water-bath that bath temperature is 60 DEG C, 50min is mixed with the revolving speed of 1100r/min with blender,
Cooled to room temperature is up to high-intensitive evenly dispersed type hydrogel.
The hydrogel that comparative example is produced with Shanghai City company is as a comparison case by high-intensitive uniform point produced by the present invention
The hydrogel dissipated in type hydrogel and comparative example detected, and testing result is as shown in table 1:
Extension test is carried out with 30mm/min on microcomputer controlled electronic universal tester, each series of samples is at least tested 3 times,
Results are averaged.
Tensile strength is the ratio of hydrogel maximum tensile stress and sample in cross section area.
The ratio of sample deformation length and its initial length when elongation at break is fracture.
1 performance measurement result of table
According to data in table 1 it is found that the evenly dispersed type hydrogel of high intensity produced by the present invention, has good mechanical performance, divides
The features such as property is good is dissipated, and preparation method is simple, it is easily operated, there is wide prospect of the application.
Claims (6)
1. a kind of preparation method of the evenly dispersed type hydrogel of high intensity, it is characterised in that specific preparation step are as follows:
(1) it weighs in 500~700g bamboo plate investment beaker, impregnates bamboo plate with sodium hydroxide solution, place the beaker water-bath
In pot, mixed liquor is made in 3~5h of constant temperature boiling, and graphite powder is added in beaker, is mixed with blender, filter is obtained by filtration
Slag, wash with distilled water filter residue 3~5 times；
(2) by after the grinding of above-mentioned filter residue and in sulfuric acid solution 1:5 in mass ratio investment three-necked flask, it is mixed that solid-liquid is made in sonic oscillation
Object is closed, the potassium permanganate powder of solidliquid mixture quality 5~8% is added into three-necked flask, is mixed with blender and oxygen is made
Change mixed liquor；
(3) hydrogen peroxide of oxidation mixed liquor quality 40~60% is added into above-mentioned three-necked flask, places the beaker permanent in water-bath
Temperature reaction, is obtained by filtration filter cake after reaction, will mix in filter cake and soybean lecithin aqueous solution 1:5 in mass ratio investment reaction kettle
Even obtained mixed serum；
(4) by mixed serum and cellulase 60:1 in mass ratio investment glass dish, glass dish is placed in climatic chamber,
Under argon atmosphere, mixed emulsion is made in 4~6h of sealing and standing, and the soybean of mixed emulsion quality 8~12% is added into glass dish
Albumen powder continues 2~3h of sealing and standing under argon atmosphere after mixing, glass dish is placed in microwave reactor after standing
Microwave treatment, then glass dish is placed in a vacuum drying oven vacuum concentration, reaction lotion is made；
(5) score meter by weight, weighs 7~9 parts of above-mentioned reaction lotions, 1~2 part of potassium peroxydisulfate, 8~10 parts of acrylamides and 20
In~22 parts of deionized water investment beakers, places the beaker in water-bath, be mixed with blender, cooled to room temperature is
Obtain high-intensitive evenly dispersed type hydrogel.
2. a kind of preparation method of the evenly dispersed type hydrogel of high intensity according to claim 1, it is characterised in that: step
(1) mass fraction of the sodium hydroxide solution described in is 10~15%, and the bath temperature of water-bath is 95~100 DEG C, thermostatted water
Boiling the time is 3~5h, and the revolving speed of blender is 400~500r/min, and mixing time is 3~4h.
3. a kind of preparation method of the evenly dispersed type hydrogel of high intensity according to claim 1, it is characterised in that: step
(2) mass fraction of the sulfuric acid solution described in is 40~50%, and supersonic frequency is 30~32kHz, and bath temperature is 5~10 DEG C,
Duration of oscillation is 3~4h, and the revolving speed of blender is 500~600r/min, and mixing time is 3~4h.
4. a kind of preparation method of the evenly dispersed type hydrogel of high intensity according to claim 1, it is characterised in that: step
(3) mass fraction of the hydrogen peroxide described in is 20~25%, and the bath temperature in water-bath is 30~35 DEG C, when isothermal reaction
Between be 30~40min, the mass fraction of soybean lecithin aqueous solution is 20~25%.
5. a kind of preparation method of the evenly dispersed type hydrogel of high intensity according to claim 1, it is characterised in that: step
(4) the sealing and standing time is 4~6h in the climatic chamber described in, and the power of microwave reactor is 700~800W, at microwave
The reason time is 10~15min, and the temperature of vacuum oven is 30~35 DEG C, and vacuum degree is 50~80Pa, and the vacuum concentration time is
100~120min.
6. a kind of preparation method of the evenly dispersed type hydrogel of high intensity according to claim 1, it is characterised in that: step
(5) bath temperature in water-bath described in is 50~60 DEG C, and the revolving speed of blender is 1000~1100r/min, and mixing is stirred
Mixing the time is 40~50min.
Priority Applications (1)
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| CN111961232A (en) * | 2020-09-09 | 2020-11-20 | 江苏江南烯元石墨烯科技有限公司 | Efficient medical graphene conductive gel and preparation method thereof |
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