CN102504117A - Aquagel with high water absorbing capacity and preparation method thereof - Google Patents
Aquagel with high water absorbing capacity and preparation method thereof Download PDFInfo
- Publication number
- CN102504117A CN102504117A CN2011102892461A CN201110289246A CN102504117A CN 102504117 A CN102504117 A CN 102504117A CN 2011102892461 A CN2011102892461 A CN 2011102892461A CN 201110289246 A CN201110289246 A CN 201110289246A CN 102504117 A CN102504117 A CN 102504117A
- Authority
- CN
- China
- Prior art keywords
- water
- absorbing capacity
- soluble monomer
- water absorbing
- high water
- 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.)
- Granted
Links
Images
Abstract
The invention discloses aquagel with high water absorbing capacity. The aquagel is prepared from the following raw materials in percentage by weight: 4-12 percent of polyvinyl alcohol, 70-90 percent of water, 5-20 percent of water-soluble monomers, 0.04-0.4 percent of an initiator and 0.03-0.3 percent of a crosslinking agent. The aquagel with high water absorbing capacity has the appearance characteristics of colorlessness and transparency, has high water absorbing capacity, and is easy for film forming. The invention further discloses a preparation method of the aquagel with high water absorbing capacity. The method comprises the following steps of: dissolving polyvinyl alcohol into a part of water under the conditions of mechanical stirring and nitrogen protection; adding a first water-soluble monomer and a part of the initiator; reacting at the temperature of 70-80 DEG C for 1-2 hours; adding the remaining water, a second water-soluble monomer, the remaining initiator and the crosslinking agent; polymerizing for 2-4 hours, and raising the temperature to 85-95 DEG C; and preserving heat for 0.5-1.5 hours, and cooling to the room temperature to obtain aquagel with high water absorbing capacity. The aquagel has the advantages of high operability, high controllability, easiness for industrial implementation, and the like.
Description
Technical field
The present invention relates to the synthetic and modification field of polymkeric substance, be specifically related to a kind of high water absorbing capacity hydrogel and preparation method thereof.
Background technology
Hydrogel be a kind of can be in water swelling, absorption and keep large quantity of moisture and don't be dissolved in the hydrophilic cross-linking polymkeric substance with three-dimensional net structure of water.Hydrogel has relatively-stationary shape, although inner water molecules is tied in the gel network, but still has certain reactivity.The special construction of this system of hydrogel is similar to the structure of organism, thereby has the behavior of similar living things system.Hydrogel has excellent biological compatibility, and has only faint effect between enzyme that is immobilized or the cell, can make the biomolecules that is fixed in the hydrogel keep the activity of long period.Because hydrogel has unique physics and chemical property, they are widely used in food-processing and preservation, agricultural with water-holding agent, women and children's sanitary product, the industrial functional materials that separates various uses such as leakproof sealing material that concentrated material, water-removal additive, construction industry use and medical dressing.
Hydrogel is of a great variety, and is different according to the polymer source of forming, and can be divided into natural polymer hydrogel and synthetic macromolecule hydrogel.Natural polymer hydrogel mainly contains starch series (starch-grafted, carboxymethylated starch etc.), Mierocrystalline cellulose series (cellulose graft, carboxymethylation Mierocrystalline cellulose etc.), protein series (Sunlover 10 class, silk-protein class etc.), other natural goodses and verivate series (pectin, alginate, chitosan etc.) thereof.The synthetic macromolecule hydrogel mainly contains ROHM and derivatives class, SEPIGEL 305 and derivatives class thereof, polyvinyl alcohol, PVP K120 class, polyepoxide class etc.Synthetic macromolecule hydrogel such as ROHM and derivatives class thereof are high because of its molecular weight, and low price and water absorbing properties get most of the attention by force, and purposes is the most extensive.
The preparation method of hydrogel mainly contains aqueous solution polymerization, inverse suspension polymerization, radiopolymerization etc.Inverse suspension polymerization needs with an organic solvent to be prone to cause environmental pollution, need increase solvent recovery unit productions in, and that product possibly have little solvent is residual, and in addition, polymeric reaction temperature is controlled when insensitive, is prone to the accident of blasting; The polymer of radiopolymerization gained has higher purity, and polyreaction can be carried out under low temperature and solid phase, and more easy to control; But radiation effect non-selectivity; Can make the reaction more complicated, need improve special radiation generating device simultaneously, and radiation have very big damaging effect to HUMAN HEALTH.The consideration of aspects such as comprehensive cost, safety, environmental protection, aqueous solution polymerization are relatively to be fit to the hydrogel preparation.
Physical strength is low and be difficult to the two big significantly shortcomings that process operation is present hydrogel, therefore is necessary hydrogel is carried out the material modification design, can improve the water-intake rate of hydrogel simultaneously.Polymer blending is a kind of important means of material modification, has become a kind of fruitful approach of polymer-modified material, appeals to day by day in recent years and payes attention to.Polymer blending is divided into two kinds of physical method and chemical processes by the preparation method.Physical method is according to the form of participating in the blend material and be divided into mechanical blending method, solution blended process and emulsion dispersion.Chemical process comprises to be utilized grafting, block copolymerization-blending method to prepare blend polymer and utilizes interpenetrating polymer networks (IPN) method to form the interpenetrating net polymer blend.The physics method is used the earliest, and technological operation is convenient, and is both economical, still accounts for critical role so far.The blend polymer performance of chemical method preparation is comparatively superior, and development was comparatively rapid in recent years.Two big shortcomings of hydrogel have determined it to be difficult for adopting the physical method modification.
And in the prior art, also all there is not high, the unmanageable technological deficiency of water-intake rate usually in the hydrogel of the method for the chemical modification of employing preparation, needs further to improve the hydrogel performance.Therefore, how to adopt the method for chemical modification, the synthetic hydrogel that has high water absorbing capacity, is prone to processing of design has great importance.
Summary of the invention
The invention provides a kind of high water absorbing capacity hydrogel, this high water absorbing capacity hydrogel has water white external appearance characteristic, water-intake rate is high and be prone to the processing film forming.
A kind of high water absorbing capacity hydrogel, process by following raw materials by weight percent:
Z 150PH 4%～12%;
Water 70%～90%;
Water-soluble monomer 5%～20%;
Initiator 0.04%～0.4%;
Linking agent 0.03%～0.3%;
Described water-soluble monomer is made up of first water-soluble monomer and second water-soluble monomer, and described first water-soluble monomer and second water-soluble monomer are identical or different.
In order better to be invented effect, the present invention is carried out preferably:
Described high water absorbing capacity hydrogel is processed by following raw materials by weight percent:
Z 150PH 4.15%～5.3%;
Water 78%～84%;
Water-soluble monomer 11%～17%;
Initiator 0.09%～0.15%;
Linking agent 0.08%～0.17%.
The present invention does not have strict requirement to the polymerization degree of Z 150PH, can select the commercially available prod for use, like the polymerization degree at 500～3000 Z 150PH.
In the present invention, the weight percent of water-soluble monomer is had strict requirement, when water-soluble monomer was adopted as 11%～17% weight percent, the high water absorbing capacity hydrogel of preparation had extra high water-intake rate.
Described first water-soluble monomer is a kind of or two or more in vinylformic acid, methylacrylic acid, acrylic amide, 2-Hydroxy ethyl acrylate, vinylformic acid-2-hydroxy propyl ester, methylacrylic acid-2-hydroxy methacrylate, the methylacrylic acid-2-hydroxy propyl ester; Described second water-soluble monomer is a kind of or two or more in vinylformic acid, methylacrylic acid, acrylic amide, 2-Hydroxy ethyl acrylate, vinylformic acid-2-hydroxy propyl ester, methylacrylic acid-2-hydroxy methacrylate, the methylacrylic acid-2-hydroxy propyl ester.Described first water-soluble monomer and second water-soluble monomer all have more hydrophilic radical as-COOH ,-OH etc., and in water, have bigger solubleness.On the one hand, first water-soluble monomer and second water-soluble monomer have more hydrophilic radical, and hydrophilic radical can form hydrogen bond with water molecules, helps to improve the rate of water absorption of final high water absorbing capacity hydrogel product; On the other hand, the preparation preferred aqueous solutions polymerization methods of hydrogel, even for making polyreaction, the monomer of reaction must have good solubility in water, promptly must be water-soluble monomer, otherwise can influence the final performance of hydrogel.
Described initiator is a kind of or two or more in ammonium persulphate, Potassium Persulphate, the Sodium Persulfate.The initiator of radical polymerization is the compound that is prone to resolve into radical; Has weak bond on the structure; Its ionic dissociation energy is 100～170kJ/mol; Far below C-C bond energy 350kJ/mol, the initiator majority is azo class and peroxide compound, like Diisopropyl azodicarboxylate, ABVN, tertbutyl peroxide, Di Cumyl Peroxide 99, BPO, peroxidized t-butyl perbenzoate, several esters of peroxy dicarbonate two rings, Potassium Persulphate, ammonium persulphate etc.The selection of initiator needs from polymerization method, polymerization temperature, many-sides such as the influence of polymer performance and accumulating stability is considered.Polymerization method is primary foundation, for aqueous solution polymerization of the present invention reaction, should select water soluble starter, and a kind of or two or more as in Potassium Persulphate, ammonium persulphate, the Sodium Persulfate etc. helps the carrying out of aqueous solution polymerization reaction of the present invention.
Described linking agent is N; N '-methylene-bisacrylamide, N, one or more in N '-methylene-bis USAF RH-1, polyethyleneglycol diacrylate, polyethylene glycol dimethacrylate, glycol diacrylate, the ethylene glycol dimethacrylate.The network structure of hydrogel plays a decisive role to water absorbing properties, and the water that is absorbed mainly is to be bound in network structure inside.According to surveying and determination, when effective chain length of grid was 10-9～10-8m, hydrogel had maximum water-intake rate.Usually, the hydrogel of Non-crosslinked does not have absorbent function on basically, and after the insignificant, water-intake rate can sharply increase, and still, can descend along with the increase of cross-linking density again after acquiring a certain degree.In order to improve the water-intake rate of high water absorbing capacity hydrogel of the present invention; Need to use linking agent; Consider that the strongly hydrophilic group is like-short the water sorption of COOH in hydrogel; Select above-mentioned linking agent for use, and the amount of linking agent has been carried out strict qualification, make the cross-linking density of high water absorbing capacity hydrogel of the present invention remain on suitable scope.
The present invention also provides a kind of preparation method of high water absorbing capacity hydrogel, is the basis with the Z 150PH, and through the means of grafting, block copolymerization-blend and IPN latex interpenetrating polymerization, the mode of employing solution polymerization is accomplished the preparation of high water absorbing capacity hydrogel.
The preparation method of described high water absorbing capacity hydrogel comprises the steps:
Under mechanical stirring and nitrogen protection condition; Z 150PH is dissolved in the portion water, adds first water-soluble monomer and part initiator, behind reaction 1h～2h under 70 ℃～80 ℃; After adding surplus water, second water-soluble monomer, residue initiator and linking agent again; Behind 70 ℃～80 ℃ polymerization 2h～4h, be warming up to 85 ℃～95 ℃, reduce to 15 ℃～35 ℃ behind insulation 0.5h～1.5h, obtain the high water absorbing capacity hydrogel.
Described water-soluble monomer can add at twice; First water-soluble monomer can be selected identical type or different types of for use with second water-soluble monomer that adds afterwards; Select methylacrylic acid-2-hydroxy methacrylate and vinylformic acid for use like first water-soluble monomer; Second water-soluble monomer is selected vinylformic acid for use, and at this moment water-soluble monomer is vinylformic acid and methylacrylic acid-2-hydroxy methacrylate.
Described part initiator is 2～3: 2 with the weight ratio of residue initiator, and described part initiator is divided into some equivalent parts, intermittently adds several times.Preferred, described part initiator is divided into 2～4 equivalent parts, and is every at a distance from intermittently equivalent adding of 25min～35min.
The weight ratio of described portion water and surplus water is 2～4: 1; The weight ratio of described first water-soluble monomer and second water-soluble monomer is 1: 1.3～3.
This polyreaction is a thermopositive reaction, and along with the increase of the water-soluble mono transformation rate and the polymerization degree, the viscosity of whole reaction system can rise rapidly.If do not adopt an effective measure the control reaction process, will have a strong impact on system inner heat transmission, mass transfer and momentum transfer, finally show as the degraded appearance and the degradation of product.Therefore, polyreaction of the present invention is carried out in two steps, simultaneously; Again the part initiator is divided into some equivalent parts, intermittently adds several times, and add the residue initiator more afterwards; Can satisfy the needs of control reaction process well, thereby make the high water absorbing capacity hydrogel of preparation have high water absorbing capacity.
The screen cloth method is adopted in described water-intake rate test, water intaking gel m
1(about 1g is accurate to 0.001), 60 ℃ of vacuum-dryings be to constant weight, weigh m
2, hydrogel water ratio k=m
1/ m
2Other is the gel m that fetches water
3(about 1g is accurate to 0.001) put in the pure water fully water absorption and swelling, the drainage that sieves weigh m
4, then xerogel water-intake rate k ' does
Described film forming testing method: water intaking gel 1g, add 10g～50g water, in 90 ℃～110 ℃ oil bath, continue to stir, left standstill 2 hours after becoming liquid, its curtain coating is being scribbled on the glass plate of silicone oil, place 80 ℃～120 ℃ oven dryings to get film.
Compared with prior art, the present invention has following advantage:
The preparation method of hydrogel provided by the invention; Adopt the method for polymer chemistry modification; At first utilize copolymerization-blend to form loose polymer network, and on Z 150PH grafting introduce hydrophilic radical (as-COOH ,-COONa etc.), increase the polarity of Z 150PH chain; Improve the consistency of blend, accelerate rate of water absorption; Utilize interpenetrating polymer networks (IPN) to make original polymer network fine and close more then, improve physical strength, participate in the polymeric hydrophilic monomer simultaneously and be uniformly distributed in the hydrogel grid, help to improve rate of water absorption and water-intake rate.That this preparation method has is workable, controllability good, be easy to advantages such as industrializing implementation.
The high water absorbing capacity hydrogel of the inventive method preparation not only has higher water-intake rate, and remedied the shortcoming of the low and difficult processing of physical strength, is easy to processing and preparing water absorbent gel film.
Description of drawings
Fig. 1 carries out the contrast optical photograph of water-intake rate test front and back for the high water absorbing capacity hydrogel of embodiment 3 preparations; Wherein, (a) being the optical photograph of the high water absorbing capacity hydrogel (water ratio k=4.5) of embodiment 3 preparations, (b) is the optical photograph of the high water absorbing capacity hydrogel of embodiment 3 preparations through water-intake rate test back (water-intake rate k '=304);
Fig. 2 is the film forming optical photograph of high water absorbing capacity hydrogel of embodiment 3 preparations.
Embodiment
The present invention combines embodiment to be further described.
Embodiment 1
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 80 ℃; Add ammonium persulphate (be 0.0338g, total consumption is 0.169g), 3.09g methylacrylic acid-2-hydroxy methacrylate and the 1.71g vinylformic acid of 1/5 amount, interval 0.5h adds the ammonium persulphate (being 0.0338g) of 1/5 amount later on.(ammonium persulphate of 1/5 amount adds 3 times reaction 1.5h altogether; Amounting to 0.1014g) back adds 30g water, N; N`-methylene-bisacrylamide (consumption is 0.185g), 14.4g vinylformic acid (degree of neutralization is 0.7) and residue ammonium persulphate (being 0.0676g); Continue reaction 2.5h at 80 ℃, be warming up to 85 ℃, reduce to 25 ℃ behind the insulation 1h and promptly get the high water absorbing capacity hydrogel product.
Embodiment 2
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 70 ℃; Add ammonium persulphate (be 0.0186g, total consumption is 0.093g), 3.09g methylacrylic acid-2-hydroxy methacrylate and the 1.71g vinylformic acid of 1/5 amount, interval 0.5h adds the ammonium persulphate (being 0.0186g) of 1/5 amount later on.(ammonium persulphate of 1/5 amount adds 3 times reaction 1.5h altogether; Amounting to 0.0558g) back adds 20g water, N; N`-methylene-bisacrylamide (consumption is 0.0822g), 6.4g vinylformic acid (degree of neutralization is 0.7) and residue ammonium persulphate (being 0.0372g); Continue reaction 2.5h at 70 ℃, be warming up to 95 ℃, reduce to 15 ℃ behind the insulation 0.5h and promptly get the high water absorbing capacity hydrogel product.
Embodiment 3
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 75 ℃; Add ammonium persulphate (be 0.0248g, total consumption is 0.124g), 3.09g methylacrylic acid-2-hydroxy methacrylate and the 1.71g vinylformic acid of 1/5 amount, interval 0.5h adds the ammonium persulphate (being 0.0248g) of 1/5 amount later on.Add 25g water, N behind the reaction 1.5h; N`-methylene-bisacrylamide (consumption is 0.123g), 9.6g vinylformic acid (degree of neutralization is 0.7) and residue ammonium persulphate (being 0.0496g); Continue reaction 3h at 75 ℃, be warming up to 85 ℃, reduce to 35 ℃ behind the insulation 1h and promptly get the high water absorbing capacity hydrogel product.
Embodiment 4
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 75 ℃; Add ammonium persulphate (be 0.0111g, total consumption is 0.0555g), 3.09g methylacrylic acid-2-hydroxy methacrylate and the 1.71g methylacrylic acid of 1/5 amount, interval 0.5h adds the ammonium persulphate (being 0.0111g) of 1/5 amount later on.Add 20g water, N behind the reaction 1.5h; N`-methylene-bisacrylamide (consumption is 0.0308g), 2.4g methylacrylic acid (degree of neutralization is 0.7) and residue ammonium persulphate (being 0.0222g); Continue reaction 3h at 75 ℃; Be warming up to 85 ℃, reduce to 25 ℃ behind the insulation 1h and promptly get the high water absorbing capacity hydrogel product.
Embodiment 5
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 80 ℃; Add the ammonium persulphate (be 0.0248g, total consumption is 0.124g) and the 4.8g methylacrylic acid-2-hydroxy methacrylate of 1/5 amount, interval 0.5h adds the ammonium persulphate (being 0.0248g) of 1/5 amount later on.Add 25g water, N behind the reaction 1.5h; N`-methylene-bisacrylamide (consumption is 0.123g), 9.6g acrylic amide and residue ammonium persulphate (being 0.0496g); Continue reaction 2.5h at 80 ℃, be warming up to 85 ℃, reduce to 25 ℃ behind the insulation 1.5h and promptly get the high water absorbing capacity hydrogel product.
Embodiment 6
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 80 ℃; Add ammonium persulphate (be 0.0248g, total consumption is 0.124g), 3.09g methylacrylic acid-2-hydroxy propyl ester and the 1.71g acrylic amide of 1/5 amount, interval 0.5h adds the ammonium persulphate (being 0.0248g) of 1/5 amount later on.Add 25g water, N behind the reaction 1.5h; N`-methylene-bisacrylamide (consumption is 0.123g), 9.6g methylacrylic acid-2-hydroxy propyl ester and residue ammonium persulphate (being 0.0496g); Continue reaction 2.5h at 80 ℃; Be warming up to 85 ℃, reduce to 25 ℃ behind the insulation 1.5h and promptly get the high water absorbing capacity hydrogel product.
Embodiment 7
Logical nitrogen in the 250ml four-hole boiling flask, and adding 60g water and 4.8g Z 150PH (PVA-124, the polymerization degree is 2450; Shanghai Aladdin company), start mechanical stirring, the time of logical nitrogen is 30min; Heat temperature raising to 80 ℃ adds ammonium persulphate (the disposable adding of ammonium persulphate of 3/5 amount, the i.e. 0.0744g of 3/5 amount; Total consumption is 0.124g), 3.09g methylacrylic acid-2-hydroxy propyl ester and 1.71g acrylic amide; Add 25g water, N behind the reaction 1.5h, N`-methylene-bisacrylamide (consumption is 0.123g), 9.6g methylacrylic acid-2-hydroxy propyl ester and residue ammonium persulphate (being 0.0496g) continue reaction 2.5h at 80 ℃; Be warming up to 85 ℃, reduce to 25 ℃ behind the insulation 1.5h and promptly get the high water absorbing capacity hydrogel product.
With the high water absorbing capacity hydrogel of embodiment 1～7 preparation, adopt the screen cloth method to carry out the water-intake rate test, concrete grammar is following: water intaking gel m
1(about 1g is accurate to 0.001), 60 ℃ of vacuum-dryings be to constant weight, weigh m
2, hydrogel water ratio k=m
1/ m
2Other is the gel m that fetches water
3(about 1g is accurate to 0.001) put in the pure water fully water absorption and swelling, the drainage that sieves weigh m
4, then xerogel water-intake rate k` does
(a) is the optical photograph of the high water absorbing capacity hydrogel (water ratio k=4.5) of embodiment 3 preparations among Fig. 1, and (b) is the optical photograph of the high water absorbing capacity hydrogel of embodiment 3 preparations through water-intake rate test back (water-intake rate k '=304) among Fig. 1.
Adopt film forming that film properties is tested: the high water absorbing capacity hydrogel 1g that gets embodiment 1～7 preparation; Add 30g water, in 100 ℃ oil bath, continue to stir, left standstill 2 hours after becoming liquid; Its curtain coating is being scribbled on the glass plate of silicone oil, placing 100 ℃ of oven dryings to get film.Fig. 2 is the film forming optical photograph of high water absorbing capacity hydrogel of embodiment 3 preparations.
Water-intake rate test data and film properties test data are as shown in table 1.
Table 1
For embodiment 4; The water-intake rate of the high water absorbing capacity hydrogel product of its preparation is lower; Mainly determine jointly by factors such as the proportioning of kind, first water-soluble monomer and second water-soluble monomer of water-soluble monomer, initiator amount, dosage of crosslinking agent; Dosage of crosslinking agent particularly, make the degree of crosslinking of high water absorbing capacity hydrogel product of preparation not enough due to.
Embodiment 6 is with embodiment 7 differences: embodiment 6 has adopted and has divided 3 equivalent to add the part initiator, and embodiment 7 has adopted disposable adding part initiator.Can be known that by table 1 embodiment 6 compares with embodiment 7, the high water absorbing capacity hydrogel of embodiment 7 preparations has more high water absorbing capacity and better film-formation result.
Claims (10)
1. high water absorbing capacity hydrogel, process by following raw materials by weight percent:
Z 150PH 4%～12%;
Water 70%～90%;
Water-soluble monomer 5%～20%;
Initiator 0.04%～0.4%;
Linking agent 0.03%～0.3%;
Described water-soluble monomer is made up of first water-soluble monomer and second water-soluble monomer, and described first water-soluble monomer and second water-soluble monomer are identical or different.
2. high water absorbing capacity hydrogel according to claim 1 is characterized in that, described high water absorbing capacity hydrogel is processed by following raw materials by weight percent:
Z 150PH 4.15%～5.3%;
Water 78%～84%;
Water-soluble monomer 11%～17%;
Initiator 0.09%～0.15%;
Linking agent 0.08%～0.17%.
3. high water absorbing capacity hydrogel according to claim 1 and 2; It is characterized in that described first water-soluble monomer is a kind of or two or more in vinylformic acid, methylacrylic acid, acrylic amide, 2-Hydroxy ethyl acrylate, vinylformic acid-2-hydroxy propyl ester, methylacrylic acid-2-hydroxy methacrylate, the methylacrylic acid-2-hydroxy propyl ester;
Described second water-soluble monomer is a kind of or two or more in vinylformic acid, methylacrylic acid, acrylic amide, 2-Hydroxy ethyl acrylate, vinylformic acid-2-hydroxy propyl ester, methylacrylic acid-2-hydroxy methacrylate, the methylacrylic acid-2-hydroxy propyl ester.
4. high water absorbing capacity hydrogel according to claim 1 and 2 is characterized in that, described initiator is a kind of or two or more in ammonium persulphate, Potassium Persulphate, the Sodium Persulfate.
5. high water absorbing capacity hydrogel according to claim 1 and 2; It is characterized in that; Described linking agent is N; N '-methylene-bisacrylamide, N, one or more in N '-methylene-bis USAF RH-1, polyethyleneglycol diacrylate, polyethylene glycol dimethacrylate, glycol diacrylate, the ethylene glycol dimethacrylate.
6. the preparation method of high water absorbing capacity hydrogel according to claim 1 and 2 is characterized in that, comprises the steps:
Under mechanical stirring and nitrogen protection condition; Z 150PH is dissolved in the portion water, adds first water-soluble monomer and part initiator, behind reaction 1h～2h under 70 ℃～80 ℃; After adding surplus water, second water-soluble monomer, residue initiator and linking agent again; Behind 70 ℃～80 ℃ polymerization 2h～4h, be warming up to 85 ℃～95 ℃, reduce to 15 ℃～35 ℃ behind insulation 0.5h～1.5h, obtain the high water absorbing capacity hydrogel.
7. the preparation method of high water absorbing capacity hydrogel according to claim 6 is characterized in that, described part initiator is 2～3: 2 with the weight ratio of residue initiator.
8. the preparation method of high water absorbing capacity hydrogel according to claim 6 is characterized in that, described part initiator is divided into some equivalent parts, intermittently adds several times.
9. the preparation method of high water absorbing capacity hydrogel according to claim 8 is characterized in that, described part initiator is divided into 2～4 equivalent parts, and is every at a distance from intermittently equivalent adding of 25min～35min.
10. the preparation method of high water absorbing capacity hydrogel according to claim 6 is characterized in that, the weight ratio of described portion water and surplus water is 2～4: 1;
The weight ratio of described first water-soluble monomer and second water-soluble monomer is 1: 1.3～3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110289246 CN102504117B (en) | 2011-09-27 | 2011-09-27 | Aquagel with high water absorbing capacity and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110289246 CN102504117B (en) | 2011-09-27 | 2011-09-27 | Aquagel with high water absorbing capacity and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102504117A true CN102504117A (en) | 2012-06-20 |
| CN102504117B CN102504117B (en) | 2013-10-30 |
Family
ID=46216256
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110289246 Active CN102504117B (en) | 2011-09-27 | 2011-09-27 | Aquagel with high water absorbing capacity and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102504117B (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102860707A (en) * | 2012-08-27 | 2013-01-09 | 上海捷儿金保温制品有限公司 | Hydrogel pad processing process |
| CN103160952A (en) * | 2013-04-15 | 2013-06-19 | 东华大学 | Preparation method of fiber with high water absorption |
| CN103709276A (en) * | 2014-01-22 | 2014-04-09 | 中国科学院长春应用化学研究所 | Super absorbent resin and preparation method thereof |
| CN106543356A (en) * | 2016-10-11 | 2017-03-29 | 华中科技大学 | A kind of hydrogel sheath and preparation method thereof |
| CN108184826A (en) * | 2017-12-28 | 2018-06-22 | 广州立白企业集团有限公司 | A kind of discoloration mosquito repellent hydrogel and preparation method thereof |
| CN108186555A (en) * | 2017-12-20 | 2018-06-22 | 华南理工大学 | Shape memory gel with calcium ion complexing and redox double-response and preparation method thereof |
| CN108659428A (en) * | 2018-05-23 | 2018-10-16 | 宁波宝亭生物科技有限公司 | A kind of preparation method of polyvinyl alcohol hydrogel |
| CN109045339A (en) * | 2018-08-29 | 2018-12-21 | 郑州工程技术学院 | A kind of medical compound antiseptic dressing and preparation method thereof |
| CN109125781A (en) * | 2018-11-16 | 2019-01-04 | 南阳市中心医院 | A kind of liver and gall surgical department's antiseptic dressing |
| CN109363185A (en) * | 2018-09-06 | 2019-02-22 | 山东禹王生态食业有限公司 | A kind of high swelling property bean dregs Process for preparing hydrogels |
| CN109385896A (en) * | 2018-11-26 | 2019-02-26 | 广东体达康医疗科技有限公司 | Novel hydrogel-cotton composite material for cooling clothes and preparation method thereof |
| CN109453418A (en) * | 2018-11-16 | 2019-03-12 | 南阳市中心医院 | A kind of vascular surgery hemostatic and antibacterial dressing |
| CN110790863A (en) * | 2019-12-05 | 2020-02-14 | 中国科学院新疆理化技术研究所 | Hydrogel with high transparency and strong acid-base stability |
| CN113376914A (en) * | 2021-05-31 | 2021-09-10 | 西南医科大学 | Stretchable microcapsule film for reflective display and preparation method thereof |
| CN113527730A (en) * | 2021-06-09 | 2021-10-22 | 安徽理工大学 | Printable composite cross-linked semipermeable membrane material, semipermeable membrane prepared from same and application of semipermeable membrane material |
| CN114940726A (en) * | 2022-06-17 | 2022-08-26 | 重庆大学锂电及新材料遂宁研究院 | Hydrogel and preparation method and application thereof |
| CN117143580A (en) * | 2023-10-27 | 2023-12-01 | 中国石油大学(华东) | Preparation method of pre-crosslinked polymer water swelling material and temporary plugging agent particles |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303716A (en) * | 1999-11-26 | 2001-07-18 | 广州市万和整形材料有限公司 | Manufacturing method of hydrogel artificial breast prosthesis |
| CN1446832A (en) * | 2003-02-08 | 2003-10-08 | 复旦大学 | Gelatin particles and preparation method |
| CN1834111A (en) * | 2006-03-10 | 2006-09-20 | 清华大学 | Process of directly synthetizing pH sensitive aquagel polymerized by UV radiation |
| CN101186706A (en) * | 2007-11-15 | 2008-05-28 | 天津大学 | Preparation method for PEG series gel nano particles |
-
2011
- 2011-09-27 CN CN 201110289246 patent/CN102504117B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303716A (en) * | 1999-11-26 | 2001-07-18 | 广州市万和整形材料有限公司 | Manufacturing method of hydrogel artificial breast prosthesis |
| CN1446832A (en) * | 2003-02-08 | 2003-10-08 | 复旦大学 | Gelatin particles and preparation method |
| CN1834111A (en) * | 2006-03-10 | 2006-09-20 | 清华大学 | Process of directly synthetizing pH sensitive aquagel polymerized by UV radiation |
| CN101186706A (en) * | 2007-11-15 | 2008-05-28 | 天津大学 | Preparation method for PEG series gel nano particles |
Non-Patent Citations (1)
| Title |
|---|
| 徐文娟等: "模糊数学在IPN型水凝胶合成中的应用", 《西南石油大学学报》, vol. 29, no. 02, 30 April 2007 (2007-04-30), pages 129 - 131 * |
Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102860707B (en) * | 2012-08-27 | 2016-03-02 | 上海捷儿金保温制品有限公司 | A kind of processing technology of hydrogel pad |
| CN102860707A (en) * | 2012-08-27 | 2013-01-09 | 上海捷儿金保温制品有限公司 | Hydrogel pad processing process |
| CN103160952A (en) * | 2013-04-15 | 2013-06-19 | 东华大学 | Preparation method of fiber with high water absorption |
| CN103160952B (en) * | 2013-04-15 | 2015-04-08 | 东华大学 | Preparation method of fiber with high water absorption |
| CN103709276A (en) * | 2014-01-22 | 2014-04-09 | 中国科学院长春应用化学研究所 | Super absorbent resin and preparation method thereof |
| CN103709276B (en) * | 2014-01-22 | 2016-06-01 | 中国科学院长春应用化学研究所 | A kind of High hydrophilous resin and its preparation method |
| CN106543356B (en) * | 2016-10-11 | 2018-11-30 | 华中科技大学 | A kind of hydrogel sheath and preparation method thereof |
| CN106543356A (en) * | 2016-10-11 | 2017-03-29 | 华中科技大学 | A kind of hydrogel sheath and preparation method thereof |
| CN108186555A (en) * | 2017-12-20 | 2018-06-22 | 华南理工大学 | Shape memory gel with calcium ion complexing and redox double-response and preparation method thereof |
| CN108186555B (en) * | 2017-12-20 | 2020-11-24 | 华南理工大学 | Shape memory hydrogel with calcium ion complexing and redox dual responses and preparation method thereof |
| CN108184826A (en) * | 2017-12-28 | 2018-06-22 | 广州立白企业集团有限公司 | A kind of discoloration mosquito repellent hydrogel and preparation method thereof |
| CN108184826B (en) * | 2017-12-28 | 2021-01-08 | 广州立白企业集团有限公司 | Color-changing mosquito-repelling hydrogel and preparation method thereof |
| CN108659428A (en) * | 2018-05-23 | 2018-10-16 | 宁波宝亭生物科技有限公司 | A kind of preparation method of polyvinyl alcohol hydrogel |
| CN109045339B (en) * | 2018-08-29 | 2021-06-11 | 郑州工程技术学院 | Medical composite antibacterial dressing and preparation method thereof |
| CN109045339A (en) * | 2018-08-29 | 2018-12-21 | 郑州工程技术学院 | A kind of medical compound antiseptic dressing and preparation method thereof |
| CN109363185A (en) * | 2018-09-06 | 2019-02-22 | 山东禹王生态食业有限公司 | A kind of high swelling property bean dregs Process for preparing hydrogels |
| CN109125781A (en) * | 2018-11-16 | 2019-01-04 | 南阳市中心医院 | A kind of liver and gall surgical department's antiseptic dressing |
| CN109453418A (en) * | 2018-11-16 | 2019-03-12 | 南阳市中心医院 | A kind of vascular surgery hemostatic and antibacterial dressing |
| CN109453418B (en) * | 2018-11-16 | 2021-09-21 | 南阳市中心医院 | Hemostatic and antibacterial dressing for vascular surgery |
| CN109385896A (en) * | 2018-11-26 | 2019-02-26 | 广东体达康医疗科技有限公司 | Novel hydrogel-cotton composite material for cooling clothes and preparation method thereof |
| CN109385896B (en) * | 2018-11-26 | 2021-06-08 | 广东体达康医疗科技有限公司 | Hydrogel-cotton composite material for cooling clothes and preparation method thereof |
| CN110790863A (en) * | 2019-12-05 | 2020-02-14 | 中国科学院新疆理化技术研究所 | Hydrogel with high transparency and strong acid-base stability |
| CN113376914A (en) * | 2021-05-31 | 2021-09-10 | 西南医科大学 | Stretchable microcapsule film for reflective display and preparation method thereof |
| CN113527730A (en) * | 2021-06-09 | 2021-10-22 | 安徽理工大学 | Printable composite cross-linked semipermeable membrane material, semipermeable membrane prepared from same and application of semipermeable membrane material |
| CN113527730B (en) * | 2021-06-09 | 2023-07-25 | 安徽理工大学 | Printable composite cross-linked semipermeable membrane material, semipermeable membrane prepared from printable composite cross-linked semipermeable membrane material and application of printable composite cross-linked semipermeable membrane material |
| CN114940726A (en) * | 2022-06-17 | 2022-08-26 | 重庆大学锂电及新材料遂宁研究院 | Hydrogel and preparation method and application thereof |
| CN117143580A (en) * | 2023-10-27 | 2023-12-01 | 中国石油大学(华东) | Preparation method of pre-crosslinked polymer water swelling material and temporary plugging agent particles |
| CN117143580B (en) * | 2023-10-27 | 2024-01-26 | 中国石油大学(华东) | Preparation method of pre-crosslinked polymer water swelling material and temporary plugging agent particles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102504117B (en) | 2013-10-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102504117B (en) | Aquagel with high water absorbing capacity and preparation method thereof | |
| Feng et al. | Synthesis and swelling behaviors of yeast-g-poly (acrylic acid) superabsorbent co-polymer | |
| CN102166399B (en) | Absorbent polymer extinguishing agent preparation method | |
| CN103804700B (en) | A kind of preparation method of photonic crystal hydrogel of chemically crosslinked of Color tunable | |
| CN102675562A (en) | Polyethylene glycol macromonomer cross-linked high-strength hydrogel and photo-initiation radical polymerization process thereof | |
| CN101519474A (en) | Double-response water gel with high swelling property and synthetic method | |
| CN106366248A (en) | Starch-based absorbent resin and preparation method therefor | |
| CN1318463C (en) | Environment responding aquogel copolymer and its prepn | |
| CN103524764B (en) | The preparation of soybean protein isolate polymer interpenetration network hydrogel and the application as medicine controlled release carrier | |
| CN101709103B (en) | Method for preparing photoresponse hydrogel containing azo monomer by utilizing light sources with different wavelengths | |
| CN104693361A (en) | Method for preparing binary copolymerized water hyacinth carboxymethyl cellulose super absorbent resin | |
| CN102391429A (en) | PH-sensitive xylan hydrogel and preparation method thereof | |
| CN103214625A (en) | Thermo-sensitive grafted hydrogel with function of resisting protein adsorption and preparation method thereof | |
| CN101974126B (en) | Method for synthesizing low-cost and super-absorbent resin from potato starch serving as raw material | |
| Sadeghi et al. | Synthesis and characterization of superabsorbent hydrogels for oral drug delivery systems | |
| CN104448145A (en) | Preparation method of super absorbent resin | |
| CN109824831A (en) | A kind of preparation method of degradable high-performance water-absorbing resin | |
| CN107056983A (en) | Prepare orthogonal regulation and control mechanical performance and medicine-releasing performance double-network hydrogel method | |
| CN102617778B (en) | A kind of synthetic method of water-keeping gel | |
| CN101974133B (en) | Method of preparing biodegradable super absorbent resin by using eggshell membrane | |
| CN105294934B (en) | A kind of high intensity anti-bacterial hydrogel and preparation method thereof | |
| CN103864980A (en) | Method for preparing agricultural super absorbent resin for ternary copolymerization | |
| JP2013049782A (en) | Gel and method of producing the same | |
| CN107099005B (en) | A kind of CO based on inierpeneirating network structure2Response type polymer microballoon and preparation method thereof | |
| CN106750013A (en) | The preparation method of organic amphiprotic copolymerized macromolecule interpenetrating networks gel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Applicant after: Zhejiang University Applicant after: Jiangsu Southern Eisai Pharmaceutical Co., Ltd. Address before: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Applicant before: Zhejiang University Applicant before: Changzhou Nanfang Sanitary Apparatus Factory Co.,Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |