CN114316098A - Attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention and synthesis process thereof - Google Patents
Attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention and synthesis process thereof Download PDFInfo
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Abstract
The invention relates to the technical field of new materials, and discloses a high water-absorbing and water-retaining attapulgite-acrylamide double-network interpenetrating hydrogel, wherein attapulgite uniformly disperses in a hydrogel matrix through chemical grafting, and a chemical crosslinking network and a double-network interpenetrating structure exist between the attapulgite and acrylamide hydrogel, so that the structural stability and the dimensional stability of the hydrogel are improved, the pore structure of the hydrogel is increased, the hydrogel can still maintain good structural stability when absorbing a large amount of water, the collapse of the three-dimensional gel network of the hydrogel is avoided, the water retention rate of the hydrogel is improved, catechol-3, 5-disulfonic acid sodium is used as a functional monomer and undergoes ring-opening esterification reaction with an anhydride group in the acrylamide hydrogel, and meanwhile, the anhydride ring-opening generates hydrophilic carboxyl groups, so that abundant carboxyl groups and sulfonic acid groups are introduced into the molecular chain of the hydrogel, the hydrophilicity and the water absorption rate of the hydrogel are obviously improved.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a high-water-absorption and water-retention attapulgite-acrylamide double-network interpenetrating hydrogel and a synthesis process thereof.
Background
The high water absorption material has excellent water absorption, salt water absorption and water retention, is widely applied to the fields of petrochemical industry, medical treatment and public health, agriculture and forestry industry and the like, the acrylamide hydrogel has a good three-dimensional hydrophilic gel network and good water absorption, and the development of novel acrylamide hydrogel becomes a research hotspot, such as double-network structure hydrogel, composite hydrogel and the like, and can improve the water absorption, water retention and mechanical strength of the hydrogel.
Compounding natural nano inorganic minerals such as diatomite, attapulgite and the like with hydrogel is an effective method for improving comprehensive performance of hydrogel, and patent CN101812157B, namely a synthetic method of poly (N-isopropylacrylamide)/attapulgite composite hydrogel, discloses compounding attapulgite poly N-isopropylacrylamide hydrogel, improving the water absorption and pore diameter of PNIPAM and improving the swelling rate, so that attapulgite and acrylamide can be prepared into composite hydrogel, and the water absorption, water retention rate, mechanical strength and other properties of the hydrogel are improved.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property and a synthesis process thereof, and the attapulgite-acrylamide double-network interpenetrating hydrogel containing carboxyl and sulfonic acid groups is synthesized, and has excellent water absorption and retention property.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property is as follows:
(1) the attapulgite-acrylamide hydrogel is added into an organic solvent and uniformly stirred, then a catalyst and catechol-3, 5-disulfonic acid sodium are added, the mixture is heated to 125 ℃ and 160 ℃ for reflux reaction for 6 to 18 hours, methanol is added for precipitation after the reaction, the mixture is filtered, deionized water and acetone are sequentially used for washing, and then the product is put into 2 to 5 percent of dilute hydrochloric acid for acidification, so that the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and water retention is obtained.
Preferably, the catalyst is p-toluenesulfonic acid (TsOH) in an amount of 1.2 to 3%.
Preferably, the organic solvent is N-methylpyrrolidone or dimethyl sulfoxide or xylene.
Preferably, the synthesis process of the attapulgite-acrylamide hydrogel is as follows:
(1) adding the nano attapulgite into a mixed acid solution of sulfuric acid and hydrochloric acid, heating to 80-95 ℃, refluxing for 6-18 h, cooling, filtering, and washing with deionized water to obtain the activated nano attapulgite.
(2) Ultrasonically dispersing the activated nano attapulgite into a dichloromethane solution, adding acryloyl chloride or methacryloyl chloride, dropwise adding a catalyst, reacting at the temperature of 20-45 ℃ for 5-10 h, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(3) Ultrasonically dispersing alkenyl modified nano attapulgite into deionized water, adding acrylamide, maleic anhydride and N, N' -Methylene Bisacrylamide (MBA), dropwise adding an initiator Ammonium Persulfate (APS) in a nitrogen atmosphere, reacting at 50-65 ℃ for 3-8 h, filtering after reaction, washing by using deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel.
Preferably, the concentration of the sulfuric acid in the mixed acid solution in the step (1) is 10-18%, and the concentration of the hydrochloric acid is 3-8%.
Preferably, the catalyst in the step (2) is pyridine, and the dosage is 12-25%.
Preferably, the mass fraction of the concavo-convex rods in the concavo-convex rod-acrylamide hydrogel in the step (3) is 4-15%.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention capacity utilizes a mixed acid solution of hydrochloric acid and sulfuric acid to carry out surface activation on attapulgite, improves the hydroxyl content on the surface of the attapulgite, introduces abundant hydroxyl, can better carry out esterification reaction with acryloyl chloride or methacryloyl chloride, thereby introducing active acryloyl oxygen groups on the surface, then carries out cross-linking polymerization with acrylamide and maleic anhydride under the initiation action of ammonium persulfate to obtain the attapulgite-grafted acrylamide composite hydrogel, attapulgite is uniformly dispersed in a hydrogel matrix through chemical grafting action, and a chemical cross-linked network and double-network interpenetrating structure exists between the attapulgite and acrylamide hydrogel, thereby improving the structural stability, dimensional stability and mechanical strength of the hydrogel, and the pore structure of the hydrogel is increased after the attapulgite and the hydrogel are compounded, under the synergistic effect, when the hydrogel absorbs a large amount of water, the hydrogel still can keep good structural stability, and the three-dimensional gel network of the hydrogel is prevented from collapsing, so that the water retention rate of the hydrogel is improved, p-toluenesulfonic acid is used as a catalyst, catechol-3, 5-disulfonic acid sodium is used as a functional monomer, and the functional monomer and an anhydride group in the acrylamide hydrogel are subjected to ring-opening esterification reaction, so that the 3, 5-disulfonic acid sodium is introduced into a hydrogel molecular chain, and the anhydride is subjected to ring-opening to generate hydrophilic carboxyl, and then the hydrophilic carboxyl and the sulfonic acid groups are introduced into the hydrogel molecular chain through acidification by hydrochloric acid, so that the hydrophilicity and the water absorption rate of the hydrogel are obviously improved, and the attapulgite-acrylamide double-network interpenetrating hydrogel shows higher water absorption rate and water retention property.
Drawings
FIG. 1 is a reaction diagram of the synthesis of an attapulgite-acrylamide hydrogel;
FIG. 2 is a reaction diagram of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: the synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property is as follows:
(1) adding the nano attapulgite into a mixed acid solution of 10-18% sulfuric acid and 3-8% hydrochloric acid, heating to 80-95 ℃, refluxing for 6-18 h, cooling, filtering, and washing with deionized water to obtain the activated nano attapulgite.
(2) Ultrasonically dispersing the activated nano attapulgite into a dichloromethane solution, adding acryloyl chloride or methacryloyl chloride, dropwise adding catalyst pyridine with the dosage of 12-25%, reacting for 5-10 h at the temperature of 20-45 ℃, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(3) Ultrasonically dispersing alkenyl modified nano attapulgite into deionized water, adding acrylamide, maleic anhydride and N, N' -Methylene Bisacrylamide (MBA), dropwise adding an initiator Ammonium Persulfate (APS) in a nitrogen atmosphere, reacting at 50-65 ℃ for 3-8 h, filtering after reaction, washing with deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel, wherein the mass fraction of the attapulgite is 4-15%.
(4) The attapulgite-acrylamide hydrogel is added into N-methyl pyrrolidone or dimethyl sulfoxide or xylene organic solvent and evenly stirred, then added with 1.2-3% of catalyst p-toluenesulfonic acid (TsOH) and catechol-3, 5-sodium disulfonate, heated to 125-160 ℃ for reflux reaction for 6-18 h, added with methanol for precipitation after reaction, filtered, washed by deionized water and acetone in sequence, and then the product is put into 2-5% diluted hydrochloric acid for acidification, thus obtaining the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and water retention.
Example 1
(1) Adding 0.5 g of nano attapulgite into 20 mL of mixed acid solution of 10% sulfuric acid and 3% hydrochloric acid, heating to 80 ℃, refluxing for 6 h, cooling, filtering, and washing with deionized water to obtain the activated nano attapulgite.
(2) Ultrasonically dispersing 0.5 g of modified nano attapulgite into 30 mL of dichloromethane solution, adding 0.4 g of acryloyl chloride, dropwise adding 0.048 g of catalyst pyridine, reacting for 5 hours at 20 ℃, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(3) Ultrasonically dispersing 0.25 g of alkenyl modified nano attapulgite into 40 mL of deionized water, adding 5 g of acrylamide, 1.2 g of maleic anhydride and 0.03 g of N, N' -methylene bisacrylamide, dropwise adding 0.2 g of initiator ammonium persulfate in a nitrogen atmosphere, reacting for 3 hours at 50 ℃, filtering after the reaction, washing by using deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel.
(4) Adding 2 g of attapulgite-acrylamide hydrogel into 50 mL of N-methylpyrrolidone solvent, uniformly stirring, adding 0.008 g of catalyst p-toluenesulfonic acid and 0.6 g of sodium catechol-3, 5-disulfonate, heating to 125 ℃, carrying out reflux reaction for 6 h, adding methanol for precipitation after reaction, filtering, washing with deionized water and acetone in sequence, and then putting the product into 2% dilute hydrochloric acid for acidification to obtain the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and water retention.
Example 2
(1) Adding 0.5 g of nano attapulgite into 40 mL of mixed acid solution of 15% sulfuric acid and 5% hydrochloric acid, heating to 80 ℃, refluxing for 6 h, cooling, filtering, and washing with deionized water to obtain the activated nano attapulgite.
(2) Ultrasonically dispersing 0.5 g of modified nano attapulgite into 40 mL of dichloromethane solution, adding 0.6 g of methacryloyl chloride, dropwise adding 0.1 g of catalyst pyridine, reacting at 45 ℃ for 5 hours, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(3) Ultrasonically dispersing 0.6 g of alkenyl modified nano attapulgite into 60 mL of deionized water, adding 5 g of acrylamide, 1.6g of maleic anhydride and 0.045 g of N, N' -methylene bisacrylamide, dropwise adding 0.25 g of initiator ammonium persulfate in a nitrogen atmosphere, reacting for 5 hours at 50 ℃, filtering after the reaction, washing by using deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel.
(4) Adding 2 g of attapulgite-acrylamide hydrogel into 70 mL of dimethyl sulfoxide solvent, uniformly stirring, adding 0.015 g of catalyst p-toluenesulfonic acid and 0.8 g of sodium catechol-3, 5-disulfonate, heating to 125 ℃, carrying out reflux reaction for 18 h, adding methanol for precipitation after reaction, filtering, washing by using deionized water and acetone in sequence, and then putting the product into 5% dilute hydrochloric acid for acidification to obtain the high-water-absorption and water-retention attapulgite-acrylamide double-network interpenetrating hydrogel.
Example 3
(1) Adding 0.5 g of nano attapulgite into 40 mL of mixed acid solution of 15% sulfuric acid and 5% hydrochloric acid, heating to 80 ℃, refluxing for 18 h, cooling, filtering, and washing with deionized water to obtain the activated nano attapulgite.
(2) Ultrasonically dispersing 0.5 g of modified nano attapulgite into 60 mL of dichloromethane solution, adding 0.7 g of acryloyl chloride, dropwise adding 0.18 g of catalyst pyridine, reacting at 35 ℃ for 8 hours, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(3) Ultrasonically dispersing 0.8 g of alkenyl modified nano attapulgite into 80 mL of deionized water, adding 5 g of acrylamide, 2 g of maleic anhydride and 0.065 g of N, N' -methylene bisacrylamide, dropwise adding 0.3 g of initiator ammonium persulfate in a nitrogen atmosphere, reacting for 5 hours at 55 ℃, filtering after reaction, washing by using deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel.
(4) Adding 2 g of attapulgite-acrylamide hydrogel into a xylene organic solvent with the volume of 120=0 mL, uniformly stirring, then adding 0.024 g of catalyst p-toluenesulfonic acid and 1.1 g of sodium catechol-3, 5-disulfonate, heating to 140 ℃, carrying out reflux reaction for 12 h, adding methanol for precipitation after the reaction, filtering, washing by using deionized water and acetone in sequence, and then putting the product into 4% diluted hydrochloric acid for acidification to obtain the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and water retention.
Example 4
(1) Adding 0.5 g of nano attapulgite into 80 mL of mixed acid solution of 18% sulfuric acid and 8% hydrochloric acid, heating to 95 ℃, refluxing for 18 h, cooling, filtering, and washing with deionized water to obtain the activated nano attapulgite.
(2) Ultrasonically dispersing 0.5 g of modified nano attapulgite into 80 mL of dichloromethane solution, adding 1 g of acryloyl chloride, dropwise adding 0.25 g of catalyst pyridine, reacting at 45 ℃ for 10 h, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(3) Ultrasonically dispersing 1.13 g of alkenyl modified nano attapulgite into 100 mL of deionized water, adding 5 g of acrylamide, 2.5 g of maleic anhydride and 0.08 g of N, N' -methylene bisacrylamide, dropwise adding 0.35 g of initiator ammonium persulfate in a nitrogen atmosphere, reacting for 8 hours at 65 ℃, filtering after the reaction, washing by using deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel.
(4) Adding 2 g of attapulgite-acrylamide hydrogel into 150 mL of xylene organic solvent, uniformly stirring, adding 0.03 g of catalyst p-toluenesulfonic acid and 1.3 g of sodium catechol-3, 5-disulfonate, heating to 160 ℃, carrying out reflux reaction for 18 h, adding methanol for precipitation after reaction, filtering, washing with deionized water and acetone in sequence, and then putting the product into 5% dilute hydrochloric acid for acidification to obtain the high-water-absorption and water-retention attapulgite-acrylamide double-network interpenetrating hydrogel.
Comparative example 1
(1) Ultrasonically dispersing 0.5 g of modified nano attapulgite into 40 mL of dichloromethane solution, adding 0.4 g of acryloyl chloride or methacryloyl chloride, dropwise adding 0.05 g of catalyst pyridine, reacting at 35 ℃ for 10 hours, filtering after the reaction, and washing by using dichloromethane and ethanol in sequence to obtain the alkenyl modified nano attapulgite.
(2) Ultrasonically dispersing 0.3 g of alkenyl modified nano attapulgite into 50 mL of deionized water, adding 5 g of acrylamide, 1.2 g of maleic anhydride and 0.03 g of N, N' -methylene bisacrylamide, dropwise adding 0.2 g of initiator ammonium persulfate in a nitrogen atmosphere, reacting for 3 hours at 55 ℃, filtering after the reaction, washing by using deionized water and ethanol in sequence, and then adding into a dialysis bag for deionized water dialysis to obtain the attapulgite-acrylamide hydrogel.
Comparative example 2
(1) Adding 5 g of acrylamide, 1.4 g of maleic anhydride and 0.04 g of N, N' -methylene bisacrylamide into 60 mL of deionized water, dropwise adding 0.2 g of initiator ammonium persulfate in a nitrogen atmosphere, reacting for 3 hours at 55 ℃, filtering after reaction, washing by using deionized water and ethanol in sequence, and then dialyzing by adding the deionized water into a dialysis bag to obtain acrylamide hydrogel.
(2) Adding 2 g of acrylamide hydrogel into 30 mL of N-methylpyrrolidone solvent, uniformly stirring, adding 0.008 g of catalyst p-toluenesulfonic acid and 0.6 g of sodium catechol-3, 5-disulfonate, heating to 140 ℃, carrying out reflux reaction for 18 h, adding methanol for precipitation after reaction, filtering, washing with deionized water and acetone in sequence, and then putting the product into 4% dilute hydrochloric acid for acidification to obtain the water-absorbent acrylamide hydrogel.
Weighing m0Adding the high-water-absorption and water-retention attapulgite-acrylamide double-network interpenetrating hydrogel of =0.2 g into 500 mL of deionized water, standing for 12 h, taking out the hydrogel, draining off the water on the surface, and weighing m1Test Water absorption Q, Q = (m)1-m0）/ m0。
Then, the hydrogel after water absorption is placed in a dark place and kept stand for 120 hours, then m2 is weighed, and the water retention rate W, W = (m)1-m2）/ m1。
| Example 1 | Example 2 | Example 3 | Example 4 | Comparison ofExample 1 | Comparative example 2 | |
| Mass m before water absorption0（g） | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Mass m after water absorption0（g） | 72.742 | 109.556 | 77.728 | 82.530 | 54.046 | 62.140 |
| Water absorption (g/g) | 362.7 | 546.8 | 397.6 | 411.7 | 269.2 | 309.7 |
| Mass m after 72 h2（g） | 53.953 | 95.313 | 69.489 | 59.982 | 28.870 | 26.554 |
| Water retention rate（%） | 69.4 | 87.0 | 89.4 | 72.7 | 53.4 | 42.7 |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A synthesis process of attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention is characterized in that: the synthesis process is as follows:
(1) the attapulgite-acrylamide hydrogel is added into an organic solvent and uniformly stirred, then a catalyst and catechol-3, 5-disulfonic acid sodium are added, the mixture is heated to 125-160 ℃ for reflux reaction for 6-18 h, and then the product is put into 2-5% diluted hydrochloric acid for acidification, so as to obtain the high water absorption and retention attapulgite-acrylamide double-network interpenetrating hydrogel.
2. The synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property according to claim 1, which is characterized in that: the catalyst is p-toluenesulfonic acid, and the dosage of the catalyst is 1.2-3%.
3. The synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property according to claim 1, which is characterized in that: the organic solvent is N-methyl pyrrolidone, dimethyl sulfoxide or xylene.
4. The synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property according to claim 1, which is characterized in that: the synthesis process of the attapulgite-acrylamide hydrogel is as follows:
(1) adding the nano attapulgite into a mixed acid solution of sulfuric acid and hydrochloric acid, heating to 80-95 ℃, and refluxing for 6-18 h to obtain activated nano attapulgite;
(2) ultrasonically dispersing the activated nano attapulgite into a dichloromethane solution, adding acryloyl chloride or methacryloyl chloride, dropwise adding a catalyst, and reacting at the temperature of between 20 and 45 ℃ for 5 to 10 hours to obtain alkenyl modified nano attapulgite;
(3) ultrasonically dispersing alkenyl modified nano attapulgite into deionized water, adding acrylamide, maleic anhydride and N, N' -methylene bisacrylamide, dropwise adding initiator ammonium persulfate in a nitrogen atmosphere, and reacting at 50-65 ℃ for 3-8 h to obtain the attapulgite-acrylamide hydrogel.
5. The synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property according to claim 4, is characterized in that: the concentration of the sulfuric acid in the mixed acid solution in the step (1) is 10-18%, and the concentration of the hydrochloric acid is 3-8%.
6. The synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property according to claim 4, is characterized in that: in the step (2), the catalyst is pyridine, and the using amount is 12-25%.
7. The synthesis process of the attapulgite-acrylamide double-network interpenetrating hydrogel with high water absorption and retention property according to claim 4, is characterized in that: the mass fraction of the concavo-convex rods in the concavo-convex rod-acrylamide hydrogel in the step (3) is 4-15%.
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| CN116768554B (en) * | 2023-05-04 | 2024-06-07 | 盐城市福奇混凝土有限公司 | Superfine mineral admixture self-compacting high-performance concrete and preparation method thereof |
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