CN113308195B - Preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology - Google Patents
Preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology Download PDFInfo
- Publication number
- CN113308195B CN113308195B CN202110792502.2A CN202110792502A CN113308195B CN 113308195 B CN113308195 B CN 113308195B CN 202110792502 A CN202110792502 A CN 202110792502A CN 113308195 B CN113308195 B CN 113308195B
- Authority
- CN
- China
- Prior art keywords
- water
- environment
- collosol
- adaptive
- hydrogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D189/00—Coating compositions based on proteins; Coating compositions based on derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention relates to the field of dyeing, in particular to a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology, which comprises the following steps: 1) preparing hydrogel matching liquid; 2) preparing collodion alum water mixed liquid; 3) and (3) preparation of environment-adaptive collosol water. The invention is based on composite phase-change hydrogel and microwave synthesis technology, can be used for various silk painting protection, and has very important practical significance for the development of the painting field and the cultural relic protection field in China.
Description
Technical Field
The invention relates to the field of pigment painting, in particular to a preparation method of environment-adaptive collosol based on composite phase-change hydrogel and microwave synthesis technology.
Background
The history of Chinese silk painting is long, and as early as a thousand years ago, ancient people learn the technology of painting mineral pigments on mature silk. When drawing, people usually use collodion alum water to treat silk cloth to ensure the firm attachment of mineral pigments. The silk painting needs to be kept in a stable environment during storage, and the aging of the silk painting can be accelerated by rapidly changing the humidity, the temperature and the pH value.
The microwave synthesis technology is a method for preparing a new material or modifying the material by inducing a chemical reaction by using microwaves to change the tissue, structure and performance of the material. The microwave reaction method has low cost, low energy consumption, high efficiency and wide application.
The hydrogel is a lightly crosslinked polymer material, and is generally a three-dimensional polymer chain network formed by combining and interweaving physical bonds and chemical bonds. By adjusting and controlling the components, the hydrogel can form sensitive and responsive behavior to a plurality of external stimuli such as temperature, humidity and pH value. The sensitive responsive phase-change hydrogel is widely applied to the fields of drug slow release, tissue engineering scaffold materials and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of environment-adaptive collosol based on composite phase-change hydrogel and microwave synthesis technology. The invention is based on a composite phase-change hydrogel mechanism, and combines an intelligent hydrogel and a collodion alum water reinforcing technology by using a microwave synthesis technology to prepare the environment-adaptive hydrogel alum water, which can effectively prevent the silk painting from aging.
The specific technical scheme of the invention is as follows: a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology comprises the following steps:
1) adding a certain amount of a cross-linking agent A, a monomer B, a composite initiator C and an additive D into deionized water, and stirring at room temperature until the cross-linking agent A, the monomer B, the composite initiator C and the additive D are completely dissolved to obtain a hydrogel matching liquid E;
2) preparing a gelatin solution under the condition of a water bath at 70-72 ℃, cooling to below 50 ℃, adding alum into the gelatin solution, stirring until the alum is completely dissolved, and cooling to obtain a collodion water matching solution F;
3) mixing the hydrogel matching liquid E obtained in the step 1) and the collosol water matching liquid F obtained in the step 2) in proportion, putting the mixture into a flask, reacting in a microwave synthesizer, and cooling to obtain the environment-adaptive collosol water G.
The preparation method of the cross-linking agent A comprises the following steps:
A) adding 2-2.2 wt% of chitosan and 1-1.2 wt% of glacial acetic acid into deionized water, and dissolving and stirring at room temperature for 1-1.1 h to prepare a sugar amine solution;
B) dropwise adding an acetone solution containing 2-3 wt% of maleic anhydride into the sugar amine solution obtained in the step A), stirring at room temperature for 4-6 hours, and reacting to synthesize maleylation chitosan;
C) and C), carrying out vacuum filtration on the maleylation chitosan obtained in the step B), precipitating with acetone, and drying in a vacuum oven at 40-45 ℃ to obtain the cross-linking agent A.
The maleylation chitosan has double bonds and can assist the monomers to generate polymerization reaction for crosslinking to form hydrogel. The hydrogel formed by crosslinking the maleylated chitosan is rich in carboxyl and amino which are sensitive to pH, and can release or accept protons in different acid-base environments to become the amphoteric pH sensitive hydrogel. The amphoteric pH sensitive hydrogel can increase swelling degree in a meta-acid/alkali environment to absorb water, and decrease swelling degree in a neutral environment to lose water, so that the influence of the change of acid and alkali in the environment on painting is relieved.
Preferably, in the step 1), the monomer B is a mixture of acrylamide and isopropyl acrylamide, and the mass ratio of the monomer B to the isopropyl acrylamide is 4: 0.9-1.1.
Hydrogels generally have water retention, while polyacrylamide hydrogels are highly sensitive to environmental humidity, and automatically adjust water content as the environment dries and humidifies. The poly (isopropyl acrylamide) hydrogel has high sensitivity to the environmental temperature, and a macromolecular chain can shrink when the temperature is higher, so that the swelling degree of the poly (isopropyl acrylamide) hydrogel can also be reduced, and the poly (isopropyl acrylamide) hydrogel can solidify pictures. The humidity/temperature sensitive hydrogel changes its form along with the change of humidity/temperature, thereby slowing down the influence of environmental change on painting.
Preferably, in the step 1), the composite initiator C is a mixed solution of tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate, and the mass ratio of the mixed solution is 2 to (0.1-0.2).
The tetramethylethylenediamine/ammonium persulfate is used as a redox initiator, can initiate polymerization at a lower reaction temperature, and has the advantages of low energy consumption and high reaction rate. Dimethyl azodiisobutyrate is azo initiator, and has the advantages of moderate activity, easy control of reaction, fast reaction rate, no residue in polymerization, no harm of decomposed product, etc. The two can play a good role in coordination as a composite initiator.
Preferably, the additive D in the step 1) is a mixture of sodium alginate, acrylic acid, ethyl acrylate and lithium chloride, and the mass ratio of the additive D to the mixture is 1 to (2.9-3.1) to (0.9-1.1) to (0.4-0.6).
Sodium alginate is a semi-interpenetrating material, and acrylamide/isopropylacrylamide polymers form an interpenetrating polymer network and keep the performances of the polymers independent. The sodium alginate has a large amount of hydrophilic groups, so that the collosol water and polymer molecular chains can form good combination without influencing the performance of the composite hydrogel. The acrylic acid and the ethyl acrylate are used as comonomers and are used for adjusting the phase transition temperature of the polyisopropylacrylamide hydrogel, and simultaneously, carboxyl is doped to adjust the pH sensitivity of the hydrogel. Lithium chloride is a metal salt dopant used to adjust the moisture sensitivity of the hydrogel. The higher the content of lithium chloride, the stronger the water absorbing capacity of the hydrogel.
Preferably, in the step 1), the molar ratio of the cross-linking agent A to the monomer B to the additive D is 5 to (29-31) to (3.9-4.1), the ratio of the addition amount of the composite initiator C to the total mass of the compounds (A + B + C) is 0.3-0.4 mL/g, and the ratio of the addition amount of the deionized water to the total mass of the compounds (A + B + C) is 13-14 mL/g.
Preferably, in the gelatin solution in the step 2), the mass fraction of gelatin is 2-2.2%, and the addition amount of alum is 0.65-0.68 g/mL.
Preferably, the volume ratio of the hydrogel mixing liquid E to the collodion water mixing liquid F in the step 3) is 1 to (8.9-9.1).
Preferably, in the reaction process of the step 3), the power of the microwave synthesizer is controlled to be 500-550W, and the reaction time is controlled to be 3-5 min.
Under the action of microwave, the monomer group is activated, the polymerization efficiency is accelerated, and the hydrogel matching liquid in the environment-adaptive collosol water can be self-polymerized in a short time.
A preparation method of environment adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology is characterized in that the use method of the environment adaptive collosol water G comprises the following steps:
1) when the cooked silk is prepared, the raw silk is placed into a 14-15% alcohol solution to be soaked and cleaned for 3-5 times, the raw silk is naturally dried and then hammered for 2-4 times, the environment-adaptive collodion alum water G is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after natural drying;
2) after painting is finished, the environment-adaptive collosol water G is uniformly coated on the painting surface, and the painting is finished after natural drying.
Preferably, the prepared environment-adaptive collosol water G is used within 20 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention uses the environment adaptive collosol alum water to treat the silk painting, and the hydrogel in the collosol alum water can respond to the change of temperature/humidity/pH value and can resist the harm of the environmental change to the silk painting.
2. The silk picture is treated by using the environment-adaptive collosol alum water, and the hydrogel can modify the collosol alum water, so that the flexibility of the silk picture is effectively improved, and the aging hazard of the silk picture is relieved.
3. The technology and the reagent used by the invention do not cause harm to human bodies and environment, and are environment-friendly.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology comprises the following steps:
1) adding 2 wt% of chitosan and 1 wt% of glacial acetic acid into deionized water, and dissolving and stirring for 1h at room temperature to prepare a sugar amine solution; dropwise adding an acetone solution containing 2 wt% of maleic anhydride into the sugar amine solution obtained in the step 1), stirring for 4 hours at room temperature, and reacting to synthesize maleylated chitosan; carrying out vacuum filtration on the maleylation chitosan obtained in the step 2), precipitating with acetone, and drying in a vacuum oven at 40 ℃ to obtain a cross-linking agent A1;
2) mixing acrylamide and isopropyl acrylamide according to the mass ratio of 4: 0.9 to obtain a monomer B1; mixing tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate according to the mass ratio of 2: 0.1 to obtain a composite initiator C1; mixing sodium alginate, acrylic acid, ethyl acrylate and lithium chloride according to the mass ratio of 1: 2.9: 0.9: 0.4 to obtain an additive D1;
3) adding 0.5g of cross-linking agent A1, 2.9g of monomer B1, 2.19mL of composite initiator C1 and 3.9g of additive D1 into 94.9mL of deionized water, and stirring at room temperature until the mixture is completely dissolved to obtain hydrogel matching liquid E1;
4) preparing a2 wt% gelatin solution under the condition of 70 ℃ water bath, cooling to 50 ℃, adding alum into the gelatin solution, wherein the addition amount of the alum is 0.65g/mL, stirring until the alum is completely dissolved, and cooling to obtain a collodion water matching solution F1;
5) taking 10mL of the hydrogel matching liquid E1 obtained in the step 3) and 89mL of the collosol water matching liquid F1 obtained in the step 4), proportionally mixing, putting into a flask, reacting in a microwave synthesizer at the power of 500W for 3min, and cooling to obtain the environment-adaptive collosol water G1.
6) The use method of the environment-adaptive collosol water G1 comprises the following steps: when the cooked silk is prepared, the raw silk is put into a 14% alcohol solution to be soaked and cleaned for 3 times, the raw silk is naturally aired and then hammered for 2 times in a positive and negative mode, the environment-adaptive collodion alum water G1 is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after the natural airing; after the painting is finished, the environment-adaptive collosol vitriol water G1 is evenly coated on the surface of the painting, and the painting is finished after being naturally dried.
Example 2:
a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology comprises the following steps:
1) adding 2.2 wt% of chitosan and 1.2 wt% of glacial acetic acid into deionized water, dissolving and stirring for 1.1h at room temperature to prepare a sugar amine solution; dropwise adding an acetone solution containing 3 wt% of maleic anhydride into the sugar amine solution obtained in the step 1), stirring for 6 hours at room temperature, and reacting to synthesize maleylated chitosan; carrying out vacuum filtration on the maleylation chitosan obtained in the step 2), precipitating with acetone, and drying in a vacuum oven at 45 ℃ to obtain a cross-linking agent A2;
2) mixing acrylamide and isopropyl acrylamide according to the mass ratio of 4: 1.1 to obtain a monomer B1; mixing tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate according to the mass ratio of 2: 0.2 to obtain a composite initiator C2; mixing sodium alginate, acrylic acid, ethyl acrylate and lithium chloride according to the mass ratio of 1: 3.1: 1.1: 0.6 to obtain an additive D2;
3) adding 0.5g of cross-linking agent A2, 3.1g of monomer B2, 3.08mL of composite initiator C2 and 4.1g of additive D2 into 107.8mL of ionized water, and stirring at room temperature until the materials are completely dissolved to obtain hydrogel matching liquid E2;
4) preparing a 2.2 wt% gelatin solution under the condition of 72 ℃ water bath, cooling to 45 ℃, adding alum into the gelatin solution, wherein the addition amount of the alum is 0.68g/mL, stirring until the alum is completely dissolved, and cooling to obtain a collodion water mixed solution F2;
5) taking 10mL of hydrogel matching liquid E2 obtained in the step 3) and 91mL of collosol water matching liquid F2 obtained in the step 4), proportionally mixing, putting into a flask, reacting in a microwave synthesizer with the power of 550W for 5min, and cooling to obtain the environment-adaptive collosol water G2.
6) The use method of the environment-adaptive collosol water G2 comprises the following steps: when the cooked silk is prepared, the raw silk is put into 15% alcohol solution to be soaked and cleaned for 5 times, the raw silk is naturally dried and then hammered for 4 times in a positive-negative mode, environment-adaptive collodion-alum water G2 is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after the natural drying; after the painting is finished, the environment-adaptive collosol vitriol water G2 is evenly coated on the surface of the painting, and the painting is finished after being naturally dried.
Example 3:
a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology comprises the following steps:
1) adding 2.1 wt% of chitosan and 1.1 wt% of glacial acetic acid into deionized water, dissolving and stirring for 1.05h at room temperature to prepare a sugar amine solution; dropwise adding an acetone solution containing 2.5 wt% of maleic anhydride into the sugar amine solution obtained in the step 1), stirring for 5 hours at room temperature, and reacting to synthesize maleylated chitosan; carrying out vacuum filtration on the maleylation chitosan obtained in the step 2), precipitating with acetone, and drying in a vacuum oven at 43 ℃ to obtain a cross-linking agent A3;
2) mixing acrylamide and isopropyl acrylamide according to the mass ratio of 4: 1 to obtain a monomer B3; mixing tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate according to the mass ratio of 2: 0.15 to obtain a composite initiator C3; mixing sodium alginate, acrylic acid, ethyl acrylate and lithium chloride according to the mass ratio of 1: 3: 1: 0.5 to obtain an additive D3;
3) adding 0.5g of cross-linking agent A3, 3g of monomer B3, 2.63mL of composite initiator C3 and 4g of additive D3 into 101.3mL of deionized water, and stirring at room temperature until the mixture is completely dissolved to obtain hydrogel matching liquid E3;
4) preparing a 2.1 wt% gelatin solution under the condition of 71 ℃ water bath, cooling to 47 ℃, adding alum into the gelatin solution, wherein the addition amount of the alum is 0.66g/mL, stirring until the alum is completely dissolved, and cooling to obtain a collodion water mixed solution F3;
5) taking 10mL of hydrogel matching liquid E3 obtained in the step 3) and 90mL of collosol water matching liquid F3 obtained in the step 4), proportionally mixing and placing into a flask, reacting in a microwave synthesizer at the power of 525W for 4min, and cooling to obtain the environment-adaptive collosol water G3.
6) The use method of the environment-adaptive collosol water G3 comprises the following steps: when the cooked silk is prepared, the raw silk is put into a 14% alcohol solution to be soaked and cleaned for 3 times, the raw silk is naturally dried and then hammered for 3 times in a positive-negative mode, the environment-adaptive collodion-alum water G3 is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after the natural drying; after the painting is finished, the environment-adaptive collosol vitriol water G3 is evenly coated on the surface of the painting, and the painting is finished after being naturally dried.
Example 4:
a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology comprises the following steps:
1) adding 2 wt% of chitosan and 1 wt% of glacial acetic acid into deionized water, and dissolving and stirring at room temperature for 1.1h to prepare a sugar amine solution; dropwise adding an acetone solution containing 2 wt% of maleic anhydride into the sugar amine solution obtained in the step 1), stirring for 5 hours at room temperature, and reacting to synthesize maleylated chitosan; carrying out vacuum filtration on the maleylation chitosan obtained in the step 2), precipitating with acetone, and drying in a vacuum oven at 50 ℃ to obtain a cross-linking agent A4;
2) mixing acrylamide and isopropyl acrylamide according to the mass ratio of 4: 1 to obtain a monomer B4; mixing tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate according to the mass ratio of 2: 0.1: 0.2 to obtain a composite initiator C4; mixing sodium alginate, acrylic acid, ethyl acrylate and lithium chloride according to the mass ratio of 1: 3: 1: 0.6 to obtain an additive D4;
3) adding 0.5g of cross-linking agent A1, 3g of monomer B1, 2.2mL of composite initiator C4 and 4g of additive D4 into 100mL of deionized water, and stirring at room temperature until the mixture is completely dissolved to obtain hydrogel matching liquid E4;
4) preparing a2 wt% gelatin solution under a water bath condition of 72 ℃, cooling to 50 ℃, adding alum into the gelatin solution, wherein the addition amount of the alum is 0.67g/mL, stirring until the alum is completely dissolved, and cooling to obtain a collodion water matching solution F4;
5) taking 20mL of hydrogel matching liquid E4 obtained in the step 3) and 180mL of collosol water matching liquid F1 obtained in the step 4), proportionally mixing, putting into a flask, reacting in a microwave synthesizer with the power of 530W and the reaction time of 5min, and cooling to obtain the environment-adaptive collosol water G4.
6) The use method of the environment-adaptive collosol water G4 comprises the following steps: when the cooked silk is prepared, the raw silk is put into 15 percent alcohol solution to be soaked and cleaned for 3 times, the raw silk is naturally aired and then hammered for 2 times in the positive and negative directions, the environment-adaptive collodion alum water G4 is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after the natural airing; after the painting is finished, the environment-adaptive collosol vitriol water G4 is evenly coated on the surface of the painting, and the painting is finished after being naturally dried.
Example 5:
a preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology comprises the following steps:
1) adding 2.2 wt% of chitosan and 1.1 wt% of glacial acetic acid into deionized water, dissolving and stirring for 1.1h at room temperature to prepare a sugar amine solution; dropwise adding an acetone solution containing 3 wt% of maleic anhydride into the sugar amine solution obtained in the step 1), stirring for 4 hours at room temperature, and reacting to synthesize maleylated chitosan; carrying out vacuum filtration on the maleylation chitosan obtained in the step 2), precipitating with acetone, and drying in a vacuum oven at 45 ℃ to obtain a cross-linking agent A5;
2) mixing acrylamide and isopropyl acrylamide according to the mass ratio of 4: 1 to obtain a monomer B5; mixing tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate according to the mass ratio of 2: 0.1: 0.2 to obtain a composite initiator C5; mixing sodium alginate, acrylic acid, ethyl acrylate and lithium chloride according to the mass ratio of 1: 3: 1: 0.4 to obtain an additive D5;
3) adding 1g of cross-linking agent A1, 6g of monomer B5, 4.5mL of composite initiator C5 and 8g of additive D5 into 200mL of deionized water, and stirring at room temperature until the materials are completely dissolved to obtain hydrogel matching liquid E5;
4) preparing a2 wt% gelatin solution under the condition of 70 ℃ water bath, cooling to 45 ℃, adding alum into the gelatin solution, wherein the addition amount of the alum is 0.65g/mL, stirring until the alum is completely dissolved, and cooling to obtain a collodion water matching solution F5;
5) taking 20mL of the hydrogel matching liquid E1 obtained in the step 3) and 180mL of the collosol water matching liquid F1 obtained in the step 4), proportionally mixing, putting into a flask, reacting in a microwave synthesizer with the power of 500W and the reaction time of 5min, and cooling to obtain the environment-adaptive collosol water G5.
6) The use method of the environment-adaptive collosol water G5 comprises the following steps: when the cooked silk is prepared, the raw silk is put into 15% alcohol solution to be soaked and cleaned for 3 times, the raw silk is naturally dried and then hammered for 3 times in a positive-negative mode, environment-adaptive collodion-alum water G5 is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after the natural drying; after the painting is finished, the environment-adaptive collosol vitriol water G5 is evenly coated on the surface of the painting, and the painting is finished after being naturally dried.
Comparative example 1
A preparation method of collosol water comprises the following steps:
1) adding 30 wt% of boiled tung oil into deionized water, dissolving and stirring for 1h at room temperature to prepare a boiled tung oil solution; dropwise adding a rosin solution containing 10 wt% into the boiled tung oil solution obtained in the step 1), and stirring for 3-4 h at the temperature of 255-265 ℃ to obtain a mixed boiled tung oil solution; precipitating the mixed boiled tung oil solution obtained in the step 2) by using acetone, and drying the mixed boiled tung oil solution in a vacuum oven at the temperature of 40 ℃ to obtain a cross-linking agent A;
2) mixing acrylamide and isopropyl acrylamide according to the mass ratio of 4: 0.9 to obtain a monomer B1; mixing tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate according to the mass ratio of 2: 0.1 to obtain a composite initiator C1; mixing sodium alginate, acrylic acid, ethyl acrylate and lithium chloride according to the mass ratio of 1: 2.9: 0.9: 0.4 to obtain an additive D1;
3) adding 0.5g of cross-linking agent A1, 2.9g of monomer B1, 2.19mL of composite initiator C1 and 3.9g of additive D1 into 94.9mL of deionized water, and stirring at room temperature until the mixture is completely dissolved to obtain hydrogel matching liquid E1;
4) preparing a2 wt% gelatin solution under the condition of 70 ℃ water bath, cooling to 50 ℃, adding alum into the gelatin solution, wherein the addition amount of the alum is 0.65g/mL, stirring until the alum is completely dissolved, and cooling to obtain a collodion water matching solution F1;
5) taking 10mL of the hydrogel matching liquid E1 obtained in the step 3) and 89mL of the collosol water matching liquid F1 obtained in the step 4), proportionally mixing, putting into a flask, reacting in a microwave synthesizer at the power of 500W for 3min, and cooling to obtain the environment-adaptive collosol water G1.
6) The use method of the environment-adaptive collosol water G1 comprises the following steps: when the cooked silk is prepared, the raw silk is put into a 14% alcohol solution to be soaked and cleaned for 3 times, the raw silk is naturally aired and then hammered for 2 times in a positive and negative mode, the environment-adaptive collodion alum water G1 is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after the natural airing; after the painting is finished, the environment-adaptive collosol vitriol water G1 is evenly coated on the surface of the painting, and the painting is finished after being naturally dried.
The examples 1 to 5 and comparative example 1 were compared with a conventional silk picture sample (comparative sample 1), and the results of the performance test were as follows.
The data in the table show that through the technical improvement, the environment adaptive collosol water can respond to the temperature/humidity/pH value change and resist the harm of the environment change to the silk painting; the environment-adaptive collosol-alum solution can effectively improve the flexibility of the silk painting and slow down the aging hazard of the silk painting. The technology and the reagent used by the invention do not cause harm to human bodies and environment, and are environment-friendly.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (6)
1. A preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology is characterized by comprising the following steps:
1) adding the cross-linking agent A, the monomer B, the composite initiator C and the additive D into deionized water, and stirring at room temperature until the cross-linking agent A, the monomer B, the composite initiator C and the additive D are completely dissolved to obtain hydrogel matching liquid E;
the preparation method of the cross-linking agent A comprises the following steps:
A) adding 2-2.2 wt% of chitosan and 1-1.2 wt% of glacial acetic acid into deionized water, and dissolving and stirring at room temperature for 1-1.1 h to prepare a sugar amine solution;
B) dropwise adding an acetone solution containing 2-3 wt% of maleic anhydride into the sugar amine solution obtained in the step A), stirring at room temperature for 4-6 hours, and reacting to synthesize maleylation chitosan;
C) carrying out vacuum filtration on the maleylation chitosan obtained in the step B), precipitating acetone, and drying in a vacuum oven at 40-45 ℃ to obtain a cross-linking agent A;
2) preparing a gelatin solution under the condition of a water bath at 70-72 ℃, cooling to below 50 ℃, adding alum into the gelatin solution, stirring until the alum is completely dissolved, and cooling to obtain a collodion water matching solution F;
3) mixing the hydrogel matching liquid E obtained in the step 1) and the collosol water matching liquid F obtained in the step 2) in proportion, placing the mixture in a container, reacting in a microwave synthesizer, and cooling to obtain environment-adaptive collosol water;
in the step 1), the monomer B is a mixture of acrylamide and isopropyl acrylamide, and the mass ratio of the monomer B to the isopropyl acrylamide is 4 (0.9-1.1); the composite initiator C is a mixed solution of tetramethylethylenediamine, ammonium persulfate and dimethyl azodiisobutyrate, and the mass ratio of the composite initiator C to the dimethyl azodiisobutyrate is 2 (0.1-0.2) to 0.1-0.2; the additive D is a mixture of sodium alginate, acrylic acid, ethyl acrylate and lithium chloride, and the mass ratio of the additive D to the additive D is 1 (2.9-3.1): (0.9-1.1): 0.4-0.6).
2. The method for preparing the environment-adaptive collosol water based on the composite phase-change hydrogel and the microwave synthesis technology in claim 1 is characterized in that the molar ratio of the cross-linking agent A, the monomer B and the additive D in the step 1) is 5 (29-31) to (3.9-4.1), the ratio of the addition amount of the composite initiator C to the total mass of the compounds (A + B + C) is 0.3-0.4 mL/g, and the ratio of the addition amount of the deionized water to the total mass of the compounds A, B and C is 13-14 mL/g.
3. The method for preparing the environment-adaptive collodion water based on the composite phase-change hydrogel and microwave synthesis technology according to claim 1, wherein in the step 2), the mass fraction of the gelatin in the gelatin solution is 2-2.2%, and the addition amount of alum is 0.65-0.68 g/mL.
4. The method for preparing the environment-adaptive collosol water based on the composite phase-change hydrogel and microwave synthesis technology according to claim 1, wherein the volume ratio of the hydrogel matching fluid E to the collosol water matching fluid F in the step 3) is 1 (8.9-9.1).
5. The method for preparing environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology according to claim 1, wherein in the reaction process of step 3), the power of a microwave synthesizer is controlled to be 500-550W, and the reaction time is controlled to be 3-5 min.
6. A method for using the colloidized water obtained by the preparation method of any one of claims 1-5, which is characterized by comprising the following steps:
1) when the cooked silk is prepared, the raw silk is placed into a 14-15% alcohol solution to be soaked and cleaned for 3-5 times, the raw silk is naturally dried and then hammered for 2-4 times, environment-adaptive collodion alum water is uniformly coated on the surface of the raw silk, and the cooked silk is obtained after natural drying;
2) after the painting is finished, the environment-adaptive collosol water is uniformly coated on the surface of the painting, and the painting is naturally dried and then is finished.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110792502.2A CN113308195B (en) | 2021-07-13 | 2021-07-13 | Preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110792502.2A CN113308195B (en) | 2021-07-13 | 2021-07-13 | Preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113308195A CN113308195A (en) | 2021-08-27 |
| CN113308195B true CN113308195B (en) | 2022-04-01 |
Family
ID=77382223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110792502.2A Active CN113308195B (en) | 2021-07-13 | 2021-07-13 | Preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113308195B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113955786B (en) * | 2021-10-28 | 2022-09-30 | 浙江大学 | Alum-based hydrogel, preparation method thereof and application thereof in energy storage |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7601355B2 (en) * | 2005-06-01 | 2009-10-13 | Northwestern University | Compositions and methods for altering immune function |
| CN101885853B (en) * | 2009-05-14 | 2012-08-29 | 天津大学 | Cured cross-linked glutinous rice flour hydrogel, preparation method and application thereof |
| CN104448161B (en) * | 2014-12-05 | 2017-02-22 | 四川大学 | Organic composite hydrogel cross-linked by modified gelatin nano-microsphere and preparation method of organic composite hydrogel |
| CN105297150A (en) * | 2015-10-30 | 2016-02-03 | 浙江理工大学 | Preparation method for simulating ancient degumming silk |
| CN105860099A (en) * | 2016-04-25 | 2016-08-17 | 宁波工程学院 | Preparation method of gelatin-based hydrogel in microwave-ultrasonic coupling field |
| CN109577088B (en) * | 2018-11-29 | 2021-05-25 | 苏州盛风文化创意发展有限公司 | Alum covering method for improving fan-shaped paper performance |
| CN109675096B (en) * | 2019-02-21 | 2021-03-12 | 武汉纺织大学 | Preparation method of chitosan fiber hydrogel dressing |
-
2021
- 2021-07-13 CN CN202110792502.2A patent/CN113308195B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113308195A (en) | 2021-08-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103554348B (en) | A kind of polymkeric substance, its preparation method and application | |
| CN102532399B (en) | Acrylic acid textile size and preparation method thereof | |
| CN107130463B (en) | A kind of interpenetrating net polymer and preparation method thereof for strengthening for paper | |
| CN113308195B (en) | Preparation method of environment-adaptive collosol water based on composite phase-change hydrogel and microwave synthesis technology | |
| DE69821584T2 (en) | Polymers for paper auxiliaries and processes for their production | |
| CN110407974B (en) | Preparation method of crosslinkable amphoteric polyacrylamide polymer | |
| CN101487207A (en) | Production method of anti-interference paper intensifier | |
| CN110591722A (en) | Preparation method of high-water-absorptivity composite resin with functions of preventing soil epidermis from shrinking and reducing water evaporation | |
| CN102627728A (en) | Preparation method for cationic chitosan graft copolymer surface sizing agent | |
| CN104761673B (en) | A kind of carbomer and preparation method thereof | |
| CN110607177A (en) | Soil water-retaining agent for saline-alkali soil and preparation method thereof | |
| KR920001039B1 (en) | Process for preparing waterswellable polymers using sodium thiosulfate as part of a redox ininiator system | |
| CN108149516A (en) | A kind of paper or paperboard grade (stock) sizing agent and preparation method thereof | |
| CN116854867A (en) | Hydrophobic association type hyperbranched papermaking wet strength agent and preparation method thereof | |
| US4275227A (en) | Synthesis of water soluble cross-linkers and their use in the manufacture of anionic polymers | |
| CN1073121C (en) | High hydroscopicity material of graft bentonite and its producing process | |
| CN1793191A (en) | Process for preparing environment protection type water retaining agent | |
| CN110669526B (en) | Preparation method of composite water-retaining agent for saline-alkali soil | |
| CN114395066A (en) | Paper moisture-proof agent and preparation method thereof | |
| JPS5938271A (en) | Water-holding agent | |
| CN106832088B (en) | A kind of nucleocapsid water lock material and its preparation method and application | |
| CN111320719A (en) | High-permeability acrylic emulsion | |
| JPH0742436B2 (en) | Method for producing aqueous coating film | |
| CN113402680B (en) | Calcium-magnesium-ion-resistant polyacrylamide and preparation method thereof | |
| CN117264109A (en) | Ionic crosslinking type low-water-potential acid-resistant agriculture and forestry water-retaining agent, and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |