CN112851979A - Preparation method and application of polyvinyl alcohol gel - Google Patents
Preparation method and application of polyvinyl alcohol gel Download PDFInfo
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Abstract
The invention discloses a preparation method and application of polyvinyl alcohol gel, which comprises the following steps: preparing a polyvinyl alcohol aqueous solution with the concentration of 5-7 wt.% under heating; heating, stirring and mixing the prepared polyvinyl alcohol aqueous solution and carboxymethyl cellulose, then adding a cross-linking agent of di (triethanolamine) diisopropyl titanate into the mixed solution of the polyvinyl alcohol and the carboxymethyl cellulose, stirring at room temperature for cross-linking reaction, and forming polyvinyl alcohol gel after the solution loses fluidity. The stability and mechanical property of the polyvinyl alcohol gel prepared by the method are greatly improved compared with the conventional polyvinyl alcohol gel formed by borax and boric acid crosslinking agents, and the gelling time of the polyvinyl alcohol gel can be accurately regulated and controlled by regulating the proportion of the polyvinyl alcohol polymer and the titanate crosslinking agent, so that the polyvinyl alcohol gel meeting various gelling time requirements can be prepared.
Description
Technical Field
The invention belongs to the field of organic polymer materials, relates to polyvinyl alcohol gel, and particularly relates to a preparation method and application of the polyvinyl alcohol gel.
Background
Polyvinyl alcohol is a water-soluble high molecular polymer, the basic structure is 1, 3-glycol, and-OH on a molecular chain can be connected with high-valence metal ions through chemical bonds to carry out a series of chemical reactions among groups, so that the polyvinyl alcohol has different functions. At present, the method for preparing polyvinyl alcohol gel is chemical crosslinking and physical crosslinking, and chemical reagents are mostly adopted for crosslinking in the field of chemical industry. According to the property of polyvinyl alcohol, two or more PVA molecules are linked together in a bridging way by a chemical crosslinking method to form a high molecular weight three-dimensional network structure wrapping free water, and the gel space network structure generally has high viscoelasticity. However, the current polyvinyl alcohol gel is limited by a cross-linking agent, so that the gelling is rapid, and the colloid is not uniform after gelling, thereby affecting the mechanical properties, stability and other properties of the colloid.
Disclosure of Invention
The invention aims to provide a preparation method of polyvinyl alcohol gel, which has controllable crosslinking time, uniform colloid and good stability.
The invention also aims to provide application of the polyvinyl alcohol gel prepared by the method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of polyvinyl alcohol gel comprises the following steps:
(1) preparing a polyvinyl alcohol aqueous solution with the concentration of 5-7 wt.% under heating;
(2) heating, stirring and mixing the polyvinyl alcohol aqueous solution prepared in the step (1) and carboxymethyl cellulose, wherein the addition amount of the carboxymethyl cellulose is 1-1.4% of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose;
(3) adding a cross-linking agent of di (triethanolamine) diisopropyl titanate into a mixed solution of polyvinyl alcohol and carboxymethyl cellulose, stirring at room temperature for cross-linking reaction, and forming polyvinyl alcohol gel after the solution loses fluidity.
Preferably, the polymerization degree and alcoholysis degree of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution in the step (1) are 2400 and 88 respectively.
Preferably, the addition amount of the cross-linking agent in the step (3) is 1.8-2.2% of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose.
The invention also provides application of the polyvinyl alcohol gel prepared by the preparation method in the aspect of plugging materials.
The polyvinyl alcohol prepared by the invention has controllable gel time and is suitable for plugging coal rock fractures.
Compared with the prior art, the invention uses di (triethanolamine) diisopropyl titanate as a cross-linking agent to carry out cross-linking reaction with polyvinyl alcohol, the titanate cross-linking agent can be cross-linked with the polyvinyl alcohol to form a net structure wrapping free water, the gelation time of the polyvinyl alcohol gel is regulated and controlled by the concentration of the cross-linking agent, so that the side chain hydroxyl of the polyvinyl alcohol molecule is fully combined with the metal ions of the cross-linking agent to form gel with uniform colloid. The polyvinyl alcohol and the carboxymethyl cellulose form intermolecular hydrogen bonds through the interaction of hydroxyl groups, and the strength of the gel is enhanced. The stability and the mechanical property of the polyvinyl alcohol gel prepared by the method are greatly improved compared with the conventional polyvinyl alcohol gel formed by borax and boric acid crosslinking agents. And the gelling time of the polyvinyl alcohol gel can be accurately regulated and controlled by adjusting the proportion of the polyvinyl alcohol polymer and the titanate crosslinking agent so as to prepare the polyvinyl alcohol gel meeting various gelling time requirements.
Drawings
FIG. 1 is a graph of gel times for polyvinyl alcohol plugging gels prepared with different cross-linking agents;
FIG. 2 is a graph of gel strength of polyvinyl alcohol plugging gels prepared with different cross-linking agents;
FIG. 3 is a graph of the swelling performance of the polyvinyl alcohol plugging gel prepared in example 3 of the present invention;
FIG. 4 is a graph of the stability performance of the polyvinyl alcohol plugging gel prepared in example 3 of the present invention;
FIG. 5 is a graph of the recovery performance of the polyvinyl alcohol plugging gel prepared in example 3 of the present invention;
FIG. 6 is a graph of the tensile properties of the polyvinyl alcohol plugging gel prepared in example 3 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
A preparation method of polyvinyl alcohol plugging gel comprises the following steps:
(1) 2488L of a polyvinyl alcohol aqueous solution having a concentration of 5 wt% was dissolved in a heating stirrer, and the solution was sealed and cooled at room temperature for 12 hours, and the viscosity of the 5 wt% 2488L polyvinyl alcohol aqueous solution was 277.5 mPas as measured by a digital viscometer.
(2) Mixing 5 wt% polyvinyl alcohol solution and carboxymethyl cellulose at 60 deg.C under stirring, wherein the addition amount of carboxymethyl cellulose is 1% of the total mass of polyvinyl alcohol and carboxymethyl cellulose, and the viscosity of the mixed solution of polyvinyl alcohol and carboxymethyl cellulose is 705 mPas measured by digital viscometer.
(3) Adding a cross-linking agent of di (triethanolamine) diisopropyl titanate into the mixed solution of the polyvinyl alcohol and the carboxymethyl cellulose, wherein the concentration of the cross-linking agent is 1.8 percent of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose, and forming polyvinyl alcohol gel after the solution loses fluidity. The gel time was recorded by a stopwatch as 103s, and the gel strength was measured by a microcomputer-controlled electronically controlled universal tester as 180.7N.
Example 2
A preparation method of polyvinyl alcohol plugging gel comprises the following steps:
(1) dissolving on a heating stirrer to prepare 2488L of polyvinyl alcohol aqueous solution, wherein the concentration of the dissolved polyvinyl alcohol aqueous solution is 6 wt%, placing at room temperature for sealing and cooling for 12h after the polyvinyl alcohol particles are completely dissolved, and measuring the viscosity of the 2488L polyvinyl alcohol aqueous solution with the concentration of 6 wt% by using a digital viscometer to be 2176.0mPa & s.
(2) Mixing a polyvinyl alcohol solution with the concentration of 6 wt% and carboxymethyl cellulose under the heating condition of 60 ℃ with stirring, wherein the addition amount of the carboxymethyl cellulose is 1.2% of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose, and the viscosity of the mixed solution of the polyvinyl alcohol and the carboxymethyl cellulose is 750 mPas measured by a digital viscometer.
(3) Adding a cross-linking agent of di (triethanolamine) diisopropyl titanate into the mixed solution of the polyvinyl alcohol and the carboxymethyl cellulose, wherein the concentration of the cross-linking agent is 2.0 percent of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose, and forming polyvinyl alcohol gel after the solution loses fluidity. The gel time was recorded by a stopwatch as 86s, and the gel strength was measured by a microcomputer-controlled electronically controlled universal tester as 247.6N.
Example 3
A preparation method of polyvinyl alcohol plugging gel comprises the following steps:
(1) dissolving 2488L of polyvinyl alcohol aqueous solution on a heating stirrer, wherein the concentration of the dissolved polyvinyl alcohol aqueous solution is 7 wt%, placing the polyvinyl alcohol particles at room temperature after being completely dissolved, sealing and cooling for 12h, and measuring the viscosity of the 2488L polyvinyl alcohol aqueous solution with the concentration of 7% by using a digital viscometer to be 2530.0 mPas.
(2) Mixing 7 wt% polyvinyl alcohol solution and carboxymethyl cellulose under stirring at 60 deg.C, wherein the addition amount of carboxymethyl cellulose is 1.4% of the total mass of polyvinyl alcohol and carboxymethyl cellulose, and the viscosity of the mixed solution of polyvinyl alcohol and carboxymethyl cellulose is 791 mPas measured by digital viscometer.
(3) Adding a cross-linking agent of di (triethanolamine) diisopropyl titanate into the mixed solution of the polyvinyl alcohol and the carboxymethyl cellulose, wherein the concentration of the cross-linking agent is 2.2 percent of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose, and forming polyvinyl alcohol gel after the solution loses fluidity. The gel time was recorded by a stopwatch as 80s, and the gel strength was measured by a microcomputer-controlled electronically controlled universal tester as 283.5N.
Example 4: preparation of polyvinyl alcohol gels with different crosslinking agents
2488L of polyvinyl alcohol aqueous solution with the concentration of 7 wt% is prepared by a heating stirrer and is respectively subjected to crosslinking reaction with boric acid, borax and a di (triethanolamine) isopropyl titanate crosslinking agent, wherein the concentrations of the crosslinking agents are respectively 1.0%, 1.5%, 2.0%, 2.5% and 3.0%, and when the polyvinyl alcohol solution is a non-flowing colloid, the final setting time is recorded by a stopwatch, and the time is the gel time. The gel strength prepared by borax, boric acid, di (triethanolamine) isopropyl titanate cross-linking agent and polyvinyl alcohol is respectively measured by a microcomputer-controlled electronic universal tester.
As is clear from fig. 1 and 2, the concentration of boric acid was increased from 1.0% to 2.5%, the gel time was 4s, and the boric acid concentration was 3.0%, the gel time was 5s, and the gel strength was increased from 60.37N to 186.77N. The concentration of borax is increased from 1.0% to 2.5%, the gel time is 3s, when the concentration of borax is 3.0%, the gel time is 4s, the gel strength is increased from 63.52N to 194.16N, and the gel strength is similar to that formed by a boric acid crosslinking agent. When the di (triethanolamine) isopropyl titanate is used as a cross-linking agent, the gel strength is increased from 85.56N to 352.03N as the concentration of TE is increased from 1.0% to 3.0% and the gel time is increased from 145s to 68s, which are higher than the gel time of boric acid and borax which are used as cross-linking agents. When borax and boric acid are used as cross-linking agents, the gelling is rapid, but the colloid strength is low and the brittleness is high. Therefore, TE is selected as the polyvinyl alcohol gel crosslinking agent.
Example 5: swelling Property test of polyvinyl alcohol gel
The swelling property of the novel polyvinyl alcohol gel is explored by adopting a liquid displacement method, and absolute ethyl alcohol is used as displacement liquid for ensuring the accuracy of data. Preparing polyvinyl alcohol gel from 7% PVA, 1.4% CMC and 2.2% TE crosslinking agent, and soaking in 200ml (V)1) Putting the beaker into a vacuum drying oven to promote the absolute ethyl alcohol to enter gel pores, and recording the total volume V of the absolute ethyl alcohol and the gel every 10min when bubbles exist in the absolute ethyl alcohol gel2. The polyvinyl alcohol gel was taken out of the absolute ethyl alcohol and the volume of the absolute ethyl alcohol remaining in the beaker was recorded as V3. After several vacuum operations, the gel was free of bubbles.
Swelling ratio of hydrogel: (V)1-V3)/(V2-V3)
As can be seen from FIG. 3, in the vacuum drying oven, the pores inside the gel are filled with air, bubbles continuously emerge under a vacuum state, the expansion rate is increased, the gel is vacuumized for 10min to 90min, the gel expansion speed is high, the expansion rate is increased from 3.7% to 16.9%, and because a pore structure exists inside the gel, when vacuumizing is started, a large amount of air in the pores escapes, a large amount of bubbles appear in the beaker, and anhydrous ethanol enters the pores of the gel under the action of pressure. And vacuumizing the gel for 90-130 min, replacing air in a part of pores of the gel with absolute ethyl alcohol, reducing bubbles emerging from the interior of the gel, and reducing the expansion rate of the gel from 17.6% to 19.7%. After the gel is vacuumized for 140min, a small amount of bubbles emerge from the gel, a small amount of air in the gel is replaced by absolute ethyl alcohol, after the gel is vacuumized for 200min, no bubbles are separated out from the gel in the beaker, pores in the gel are completely filled with the absolute ethyl alcohol, the expansion rate of the gel is 21.5%, and after the gel is continuously vacuumized, the gel is kept stable and does not expand any more.
Example 6: stability testing of polyethylene gels
The network structure of gel wraps up a large amount of moisture, and the network space structure difference of gel can be represented to a certain extent to the water content of gel, and the gel water content that different application range needs is different, and in the aspect of splitting shutoff, gel service time can be prolonged to the gel of high water content. The method for measuring the water content of the gel usually adopts an intuitive gel heating and weighing method, the concentration of the polyvinyl alcohol is 7 percent, the concentration of the CMC is 1.4 percent, the concentration of the cross-linking agent is changed to be 1.8 percent, 2.0 percent, 2.2 percent, 2.4 percent and 2.6 percent to prepare the PVA gel, and the PVA gel is weighed by a balance to obtain the mass m. Then putting the gel into a vacuum drying oven, setting the temperature of the vacuum drying oven at 40 ℃, drying for 24 hours, weighing the mass of the gel on an electronic balance until the mass is constant, and recording the mass of the dried gel as m0The mass fraction of water in the gel is as follows:
W＝(m-m0)/m*100
as can be seen from fig. 4, the water content of the polyvinyl alcohol gel increases with the increase of the TE concentration of the cross-linking agent, and the water content of the gel is 81.50%, 84.82%, 86.15%, 87.09%, 87.83% when the concentration of the cross-linking agent is 1.8%, 2.0%, 2.2%, 2.4%, 2.6%, and the concentration of the cross-linking agent is increased, so that the increase of the concentration of the cross-linking agent can be combined with more cross-linking sites of the polyvinyl alcohol molecules, so that the skeleton structure of the gel wraps more water molecules, and the water content of the. The polyvinyl alcohol molecules contain a large amount of hydroxyl, the number of hydrogen bonds formed between the water molecules and the hydroxyl groups of the polyvinyl alcohol molecules is increased due to the increase of the water content, the gel volume is expanded, the distance between polyvinyl alcohol molecular chains is increased, partial hydrogen bonds formed between the hydroxyl groups of the polyvinyl alcohol molecules are destroyed, the molecular chain movement is accelerated, the collision probability between the polyvinyl alcohol molecules is increased, and more free water is fixed in a molecular skeleton.
Example 7: return Performance test of polyvinyl alcohol gel
In order to test the recovery performance of the polyvinyl alcohol gel of the plugging material, the polyvinyl alcohol gel is prepared according to the optimal proportion (7% of PVA, 1.4% of CMC and 2.2% of TE cross-linking agent), the prepared gel sample is 25mm by 30mm, the polyvinyl alcohol gel is compressed at the compression speed of 2mm/min through a microcomputer controlled electronic universal tester, the compression recovery performance of the polyvinyl alcohol gel is tested, and the compression rate of the gel is 20%, 50% and 70%. The gel was compressed continuously 20%, 50% and 70%, and the number of times of compression was 10, and the compressibility of each time was calculated.
As can be seen from fig. 5: after the polyvinyl alcohol gel is compressed by 20%, 50% and 70%, a certain pressure difference exists before and after the gel recovers, but the pressure difference distance is small, and the good recovery performance of the gel is shown. Theoretically, the gel can be completely recovered after being compressed, because the hydroxyl of the polyvinyl alcohol molecule and TE are crosslinked to form a net structure, the net structure has certain elasticity and flexibility, the gel becomes an elastomer, the polyvinyl alcohol gel molecular chain needs a certain time to be expanded again after being compressed, the time provided by the microcomputer-controlled electronic universal testing machine is not enough to expand the gel molecular chain, so that the molecular chain is recovered, the polyvinyl alcohol gel is stood for a period of time, the microcomputer-controlled electronic universal testing machine is used for testing again, the compression curves are basically overlapped, and the shape is basically and completely recovered.
Example 8: tensile Property test of polyvinyl alcohol gel
Putting the polyvinyl alcohol gel prepared in the example 3 into a vacuum drying oven, drying for 6h at 60 ℃, weighing the dried gel sample by an electronic balance, preparing the dried PVA sample into a sheet of 150mm by 40mm by 2mm when the constant weight of the gel sample shows that the moisture of the gel is completely evaporated, and electronically testing the tensile property of the gel by a microcomputer-controlled electronic universal tester, wherein the applied testing force of the gel is 5mm/min, and the gel testing standard is the tensile standard of the high polymer porous material.
As can be seen from FIG. 6, when the pulling force is applied for 0-32s, the gel stretching force of the polyvinyl alcohol increases with time, the stretching force increases from 0N to 15N, the network structure of the gel is stretched, and the stretching rate increases rapidly due to the elasticity of the gel itself. When the time of applying the pulling force is between 32s and 38s, the pulling rate is slowed down due to the strength and the toughness of the gel, the pulling force value of the gel is 15N, the pulling force is kept unchanged, the acting force among gel molecules forms a barrier to the pulling force, and the pulling force is kept uniform. When the pulling force is applied for a time of 39s-75s, the gel stretching force is increased from 15N to 23N, and the increase rate is reduced. When the pulling force is applied for 75-80 s, the toughness of the three-dimensional structure of the gel is maximized, the pulling force of the gel is 23N, the gel is kept unchanged, after the pulling force is applied for 80s, the pulling force value of the gel is reduced, the three-dimensional structure of the gel is damaged, the acting force between gel molecules and a cross-linking agent is not enough to offset the pulling force, and the gel breaks until the gel is broken.
Claims (4)
1. A preparation method of polyvinyl alcohol gel is characterized by comprising the following steps:
(1) preparing a polyvinyl alcohol aqueous solution with the concentration of 5-7 wt.% under heating;
(2) heating, stirring and mixing the polyvinyl alcohol aqueous solution prepared in the step (1) and carboxymethyl cellulose, wherein the addition amount of the carboxymethyl cellulose is 1-1.4% of the total mass of the polyvinyl alcohol and the carboxymethyl cellulose;
(3) adding a cross-linking agent of di (triethanolamine) diisopropyl titanate into a mixed solution of polyvinyl alcohol and carboxymethyl cellulose, stirring at room temperature for cross-linking reaction, and forming polyvinyl alcohol gel after the solution loses fluidity.
2. The method of claim 1, wherein the degree of polymerization and alcoholysis of the polyvinyl alcohol in the aqueous solution of polyvinyl alcohol in step (1) is 2400.
3. The method for preparing polyvinyl alcohol gel according to claim 1, wherein the amount of the crosslinking agent added in step (3) is 1.8% -2.2% of the total mass of polyvinyl alcohol and carboxymethyl cellulose.
4. Use of the polyvinyl alcohol gel prepared by the preparation method according to any one of claims 1 to 3 in plugging materials.
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| CN115181383A (en) * | 2022-08-19 | 2022-10-14 | 扬州大学 | Preparation method of stimulus-responsive hydrogel |
| US12127469B2 (en) * | 2022-11-29 | 2024-10-22 | E Ink Corporation | Multi-layer device comprising a repair layer having conductive a hydrogel film or beads |
| CN116042200A (en) * | 2022-12-23 | 2023-05-02 | 中国水利水电第七工程局成都水电建设工程有限公司 | Delay crosslinking water shutoff gel |
| CN118267517A (en) * | 2024-06-03 | 2024-07-02 | 山东永聚医药科技股份有限公司 | Antibacterial hydrogel wound dressing and preparation method thereof |
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