CN103087252B - Preparation method of high-absorption composite - Google Patents
Preparation method of high-absorption composite Download PDFInfo
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- CN103087252B CN103087252B CN201310015645.8A CN201310015645A CN103087252B CN 103087252 B CN103087252 B CN 103087252B CN 201310015645 A CN201310015645 A CN 201310015645A CN 103087252 B CN103087252 B CN 103087252B
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Abstract
The invention discloses a preparation method of a high-absorption composite. The preparation method comprises the following steps: 1) fully mixing acrylamide monomer, macromolecular surfactant, water and indianite, and filtering to obtain modified indianite; 2) preparing acrylic acid into water solution with mass concentration of 50-60%, adding an adsorbent, evenly mixing, filtering to remove a polymerization inhibitor, and neutralizing the filtrate by sodium hydroxide to obtain acrylic acid neutralization solution; and 3) adding the acrylamide monomer, the modified indianite, a crosslinking agent and an initiator at room temperature, fully mixing, increasing the temperature of the mixture to 70-85 DEG C for full reaction to obtain gel, and then drying, breaking, grinding and screening the gel. Compared with the high-absorption material prepared without addition of the indianite, the high-absorption composite prepared by adopting the method is obviously improved in absorption speed, water retaining capacity and pressurized absorbed capacity, can meet the requirement of sanitary materials, and is obviously shortened in drying time.
Description
Technical field
The present invention relates to a kind of preparation method of high water absorption composite material.
Background technology
High absorbency material mainly refers to polymer super absorbent resin, refer to there is wetting ability but the multiphase gel system that formed of the water that water-fast crosslinked polymer network absorbs own wt several times and even hundreds of times thousands of times, be widely used in the fields such as the sanitary material such as sanitary napkin, baby paper diaper, drought-resistant water-preserving, agricultural gardening, bio-medical, along with making rapid progress of scientific and technological level and improving constantly of people's living standard, its Application Areas constantly expands, and penetrates into the every field of industrial production and people's life gradually.High absorbency material has polyacrylic acid and copolymerization high absorbency material, polyacrylamide and copolymerization high absorbency material thereof, Mierocrystalline cellulose or starch-grafted high absorbency material, polyvinyl alcohol high absorbency material etc. by composition main species, the high absorbency material of different preparation method, different composition also difference to some extent in performance, Application Areas etc.
The high absorbency material being applied to sanitary material, because it is direct and human contact, is considered the impact on human body skin and organ, in biocompatibility, absorption rate, pressurizing absorption amount etc., is had higher requirement.The high absorbency material being applied to sanitary material is at present mainly vinylformic acid and multipolymer high absorbency material thereof, the preparation method adopted is primarily of inverse suspension method and solution polymerization process, inverse suspension method needs with an organic solvent owing to existing, complex manufacturing, be difficult to realize the shortcomings such as continuous prodution be difficult to popularize, mostly adopt solution polymerization process at present, but solution polymerization process obtain product performance be difficult to compared with inverse suspension method product, absorption rate particularly required by sanitary material, water-retaining capacity and pressurization water regain often need just can meet the demands through aftertreatment.In addition, the drying of polyacrylic resin that prepared by solution polymerization process is also a large technical barrier.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high water absorption composite material.
The technical solution used in the present invention is:
A preparation method for high water absorption composite material, comprises the following steps:
1) acrylamide monomer, polymeric surface active agent, water, halloysite are mixed fully, filter, obtain modification halloysite;
2) Acrylic Acid Monomer is made the aqueous solution that mass concentration is 50-60%, add the sorbent material of Acrylic Acid Monomer quality 1%, mix, filter and remove stopper, filtrate neutralizes with sodium hydroxide, obtains vinylformic acid neutralizer;
3) under room temperature, acrylamide monomer, modification halloysite, linking agent, initiator is added in the vinylformic acid neutralizer that upper step obtains, abundant mixing, fully react mixture being warmed up to 70-85 DEG C, obtain gel, then gel is dried at 120-140 DEG C constant weight, fragmentation, pulverizes, sieves;
In step 1), the quality of acrylamide monomer is the 5%-10% of halloysite quality, and the quality of polymeric surface active agent is the 0.1%-0.5% of halloysite quality, and the consumption of water is the 500%-2000% of halloysite quality;
Step 2) in, sodium hydroxide is 0.6-0.8 with the ratio of the amount of substance of Acrylic Acid Monomer;
In step 3), the consumption of acrylamide monomer is step 2) in the 10%-30% of Acrylic Acid Monomer quality, the consumption of modification halloysite is step 2) in Acrylic Acid Monomer quality 1 ~ 6%, the consumption of linking agent is step 2) in the 0.2%-1% of Acrylic Acid Monomer quality, initiator amount is step 2) in the 0.1%-0.5% of Acrylic Acid Monomer quality.
Described polymeric surface active agent is the one in polyvinylpyrrolidone PVPK12, polyvinylpyrrolidone PVPK15, polyoxyethylene glycol PEG400, polyoxyethylene glycol PEG600.
Described sorbent material is gas-phase silica or gac.
Described linking agent is N, N ,-methylene-bisacrylamide, N, N, the one of-diallyl tartardiamide, ethylene glycol diacrylate.
Described initiator is the one in benzoyl peroxide, Diisopropyl azodicarboxylate, Potassium Persulphate.
The whiteness of described halloysite is greater than 90.
The invention has the beneficial effects as follows: the present invention adopts reactive monomer acrylamide and polymeric surface active agent to carry out surface coating modification to halloysite and obtains modification halloysite, and then by realizing the reactive composite of modification halloysite and polymkeric substance in the process of vinylformic acid, acrylamide monomer copolymerzation with cross-linking, finally prepare high water absorption composite material.
Compare with the high absorbency material do not added prepared by halloysite, prepared high water absorption composite material not only absorption rate, water-retaining capacity and pressurizing absorption amount significantly improves, and can meet sanitary material requirement, meanwhile, time of drying also obviously shortens.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1:
(1) acrylamide monomer, polymeric surface active agent are dissolved in distilled water, stir, then add high white halloysite (whiteness is greater than 90), stir 2 hours at 30 DEG C, filter, obtain modification halloysite.
Wherein, acrylamide monomer is 6% of halloysite quality, and polymeric surface active agent is polyvinylpyrrolidone (PVPK15), and consumption is 0.2% of halloysite quality, and distilled water consumption is 1000% of halloysite quality.
(2) vinylformic acid is dissolved in distilled water, makes the acrylic acid solution that mass concentration is 60%, add gac by 1% of Acrylic Acid Monomer quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein.Add in remaining filtrate sodium hydroxide carry out in and, obtain vinylformic acid neutralizer,
Wherein, sodium hydroxide is 0.8 with the ratio of the amount of substance of Acrylic Acid Monomer;
(3) in aforesaid propylene acid neutralizer, acrylamide monomer, modification halloysite, linking agent, initiator is added, now stir at normal temperatures and obtain reaction solution in 0.5 hour, then reaction solution is transferred in tetrafluoroethylene reaction tray, at 75 DEG C, reaction obtains gel in 0.5 hour, constant weight is dried at 120 DEG C, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object high water absorption composite material product.
In step (3), the consumption of acrylamide monomer is 10% of Acrylic Acid Monomer quality in step (2), the consumption of modification halloysite is 6% of Acrylic Acid Monomer quality in step (2), linking agent is ethylene glycol diacrylate, consumption is 0.3% of Acrylic Acid Monomer quality in step (2), initiator is benzoyl peroxide, and consumption is 0.2% of Acrylic Acid Monomer quality in step (2).
comparing embodiment 1:
Do not add modification halloysite, namely all the other steps only need adopt step (2), (3), without modification halloysite in step (3) with embodiment 1().
embodiment 2:
(1) acrylamide monomer, polymeric surface active agent are dissolved in distilled water, stir, then add high white halloysite (whiteness is greater than 90), stir 1 hour at 50 DEG C, filter, obtain modification halloysite.
Wherein, acrylamide monomer is 10% of halloysite quality, and polymeric surface active agent is polyoxyethylene glycol (PEG600), and consumption is 0.5% of halloysite quality, and distilled water consumption is 2000% of halloysite quality.
(2) vinylformic acid is dissolved in distilled water, makes the acrylic acid solution that mass concentration is 50%, add gas-phase silica by 1% of Acrylic Acid Monomer quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein.Add in remaining clear liquid sodium hydroxide carry out in and, obtain vinylformic acid neutralizer,
Wherein, sodium hydroxide is 0.7 with the ratio of the amount of substance of Acrylic Acid Monomer;
(3) in aforesaid propylene acid neutralizer, acrylamide monomer, modification halloysite, linking agent, initiator is added, now stir at normal temperatures and obtain reaction solution in 0.5 hour, then reaction solution is transferred in tetrafluoroethylene reaction tray, at 80 DEG C, reaction obtains gel in 0.5 hour, constant weight is dried at 130 DEG C, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object high water absorption composite material product.
In step (3), the consumption of acrylamide monomer is 20% of Acrylic Acid Monomer quality in step (2), and the consumption of modification halloysite is 2% of Acrylic Acid Monomer quality in step (2), and linking agent is N, N
,-methylene-bisacrylamide, consumption is 0.5% of Acrylic Acid Monomer quality in step (2), and initiator is Diisopropyl azodicarboxylate, and consumption is 0.3% of Acrylic Acid Monomer quality in step (2).
comparing embodiment 2:
Do not add modification halloysite, namely all the other steps only need adopt step (2), (3), without modification halloysite in step (3) with embodiment 2().
embodiment 3:
(1) acrylamide monomer, polymeric surface active agent are dissolved in distilled water, stir, then add the high white halloysite (whiteness is greater than 90) of high-quality of tubulose, stir 1.5 hours at 40 DEG C, filter, obtain modification halloysite.
Wherein, acrylamide monomer is 8% of halloysite quality, and polymeric surface active agent is polyvinylpyrrolidone (PVPK12), and consumption is 0.3% of halloysite quality, and distilled water consumption is 1500% of halloysite quality.
(2) vinylformic acid is dissolved in distilled water, makes the acrylic acid solution that mass concentration is 55%, add gac by 1% of Acrylic Acid Monomer quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein.Add in remaining clear liquid sodium hydroxide carry out in and, obtain vinylformic acid neutralizer,
Wherein, sodium hydroxide is 0.6 with the ratio of the amount of substance of Acrylic Acid Monomer;
(3) in aforesaid propylene acid neutralizer, acrylamide monomer, modification halloysite, linking agent, initiator is added, now stir at normal temperatures and obtain reaction solution in 0.5 hour, then reaction solution is transferred in tetrafluoroethylene reaction tray, at 70 DEG C, reaction obtains gel in 0.5 hour, constant weight is dried at 140 DEG C, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object high water absorption composite material product.
In step (3), the consumption of acrylamide monomer is 30% of Acrylic Acid Monomer quality in step (2), and the amount of modification halloysite is 4% of Acrylic Acid Monomer quality in step (2), and linking agent is N, N
,-diallyl tartardiamide, consumption is 0.8% of Acrylic Acid Monomer quality in step (2), and initiator is Potassium Persulphate, and consumption is 0.5% of Acrylic Acid Monomer quality in step (2).
comparing embodiment 3:
Do not add modification halloysite, namely all the other steps only need adopt step (2), (3), without modification halloysite in step (3) with embodiment 3().
The performance test results of above-described embodiment and comparing embodiment is as table 1:
table 1: the effect of embodiment and comparing embodiment
illustrate:
performance test methods of the present invention is as follows:
Suck ionized water multiple (g/g): with reference to " People's Republic of China's agricultural industry criteria " (NY886-2004).
Absorbed dose (g/g): with reference to " National Standard of the People's Republic of China " (GB/T22905-2008).
Water-retaining capacity (g/g): with reference to " National Standard of the People's Republic of China " (GB/T22905-2008).
Pressurizing absorption amount (g/g): with reference to " National Standard of the People's Republic of China " (GB/T22905-2008).
Absorption rate (s): with reference to " National Standard of the People's Republic of China " (GB/T22875-2008).
effect analysis:
As can be seen from the result of above-described embodiment, compare with the polyacrylic high absorbency material do not added prepared by halloysite, high water absorption composite material prepared by the inventive method sucks ionized water multiple and decreases, but has no significant effect for the use of sanitary material.Although absorbed dose decreases, water-retaining capacity, absorption rate and pressurizing absorption amount significantly improve, and can meet sanitary material requirement, and meanwhile, time of drying obviously shortens, and can enhance productivity, reduce production cost.
Claims (6)
1. a preparation method for high water absorption composite material, is characterized in that: comprise the following steps:
1) acrylamide monomer, polymeric surface active agent, water, halloysite are mixed fully, filter, obtain modification halloysite;
2) Acrylic Acid Monomer is made the aqueous solution that mass concentration is 50-60%, add the sorbent material of Acrylic Acid Monomer quality 1%, mix, filter and remove stopper, filtrate neutralizes with sodium hydroxide, obtains vinylformic acid neutralizer;
3) under room temperature, acrylamide monomer, modification halloysite, linking agent, initiator is added in the vinylformic acid neutralizer that upper step obtains, abundant mixing, mixture is warmed up to 70-85 DEG C more fully to react, obtain gel, then gel is dried at 120-140 DEG C constant weight, fragmentation, pulverizes, sieves;
In step 1), the quality of acrylamide monomer is the 5%-10% of halloysite quality, and the quality of polymeric surface active agent is the 0.1%-0.5% of halloysite quality, and the consumption of water is the 500%-2000% of halloysite quality;
Step 2) in, sodium hydroxide is 0.6-0.8 with the ratio of the amount of substance of Acrylic Acid Monomer;
In step 3), the consumption of acrylamide monomer is step 2) in the 10%-30% of Acrylic Acid Monomer quality, the consumption of modification halloysite is step 2) in Acrylic Acid Monomer quality 1 ~ 6%, the consumption of linking agent is step 2) in the 0.2%-1% of Acrylic Acid Monomer quality, initiator amount is step 2) in the 0.1%-0.5% of Acrylic Acid Monomer quality.
2. the preparation method of a kind of high water absorption composite material according to claim 1, is characterized in that: described polymeric surface active agent is the one in polyvinylpyrrolidone PVPK12, polyvinylpyrrolidone PVPK15, polyoxyethylene glycol PEG400, polyoxyethylene glycol PEG600.
3. the preparation method of a kind of high water absorption composite material according to claim 1, is characterized in that: described sorbent material is gas-phase silica or gac.
4. the preparation method of a kind of high water absorption composite material according to claim 1, is characterized in that: described linking agent is N, N
,-methylene-bisacrylamide, N, N
,the one of-diallyl tartardiamide, ethylene glycol diacrylate.
5. the preparation method of a kind of high water absorption composite material according to claim 1, is characterized in that: described initiator is the one in benzoyl peroxide, Diisopropyl azodicarboxylate, Potassium Persulphate.
6. the preparation method of a kind of high water absorption composite material according to claim 1, is characterized in that: the whiteness of described halloysite is greater than 90.
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| CN107216429A (en) * | 2017-07-11 | 2017-09-29 | 徐州诺克非医药科技有限公司 | A kind of composite high-performance absorbent material preparation method |
| CN107320244A (en) * | 2017-09-01 | 2017-11-07 | 徐州诺克非医药科技有限公司 | A kind of lace-tied type high water absorption type paper diaper |
| CN108479728B (en) * | 2018-03-21 | 2021-06-22 | 浙江理工大学 | Composite drying agent based on quicklime waste residues and preparation method thereof |
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| CN1746216A (en) * | 2005-06-24 | 2006-03-15 | 华南理工大学 | Preparation of polymer composite material from halloysite nanometer tube |
| CN101712779A (en) * | 2009-08-25 | 2010-05-26 | 上海普利特复合材料股份有限公司 | Polypropylene nano composite material and preparation method thereof |
| CN101874274A (en) * | 2007-11-27 | 2010-10-27 | 玛丽亚·斯特罗姆 | Composite materials including an intrinsically conducting polymer, and methods and devices |
| CN102580696A (en) * | 2012-02-20 | 2012-07-18 | 江苏大学 | Preparation method of temperature sensitive adsorbent of halloysite magnetic composite material surface blotting |
| CN102644214A (en) * | 2012-04-12 | 2012-08-22 | 华南理工大学 | Preparation method and application of polyacrylamide/keramite nanotube composite papermaking filler |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1746216A (en) * | 2005-06-24 | 2006-03-15 | 华南理工大学 | Preparation of polymer composite material from halloysite nanometer tube |
| CN101874274A (en) * | 2007-11-27 | 2010-10-27 | 玛丽亚·斯特罗姆 | Composite materials including an intrinsically conducting polymer, and methods and devices |
| CN101712779A (en) * | 2009-08-25 | 2010-05-26 | 上海普利特复合材料股份有限公司 | Polypropylene nano composite material and preparation method thereof |
| CN102580696A (en) * | 2012-02-20 | 2012-07-18 | 江苏大学 | Preparation method of temperature sensitive adsorbent of halloysite magnetic composite material surface blotting |
| CN102644214A (en) * | 2012-04-12 | 2012-08-22 | 华南理工大学 | Preparation method and application of polyacrylamide/keramite nanotube composite papermaking filler |
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