CN106543385A - A kind of preparation method of pH responsive types semi-interpenetrating network aqueous gel - Google Patents
A kind of preparation method of pH responsive types semi-interpenetrating network aqueous gel Download PDFInfo
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- CN106543385A CN106543385A CN201610750344.3A CN201610750344A CN106543385A CN 106543385 A CN106543385 A CN 106543385A CN 201610750344 A CN201610750344 A CN 201610750344A CN 106543385 A CN106543385 A CN 106543385A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/14—Soil-conditioning materials or soil-stabilising materials containing organic compounds only
- C09K17/18—Prepolymers; Macromolecular compounds
- C09K17/32—Prepolymers; Macromolecular compounds of natural origin, e.g. cellulosic materials
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Abstract
The invention belongs to water-loss reducer of soil preparation field, and in particular to a kind of preparation method of pH responsive types semi-interpenetrating network aqueous gel.Step of the present invention includes:(1) butt starch is placed in there-necked flask, plus appropriate distilled water, after gelatinizing in water-bath, obtain gelatinized corn starch;(2) poly-aspartate is weighed by formula ratio, be dissolved in appropriate distilled water, obtain poly-aspartate solution, appropriate acrylic acid is slowly dropped in poly-aspartate solution the mixture for obtaining acrylic acid and poly-aspartate after stirring;(3) mixture by acrylic acid with poly-aspartate is added in the gelatinized corn starch of step (1), after mixing, sequentially adds initiator potassium persulfate, sodium sulfite and cross-linking agent methylene-bisacrylamide;(4) after reactant plastic, blob of viscose is cut into, puts in tap water and soak, wash away unreacted monomer, initiator and cross-linking agent, sample is washed to neutrality, drying, crushed and sieve, obtain pH sensitivity semi-interpenetrating network aqueous gel finished products.
Description
Technical field
The invention belongs to soil water-retaining technical field of material, and in particular to a kind of pH responsive types semi-intercrossing network water-setting
The preparation method of glue.
Background technology
China's water resource lacks, rainwater skewness, and the shortage of soil moisture has a strong impact on the production of agricultural and forestry.
Water-loss reducer of soil can pass through to improve absorbability of the soil to natural rainfall and man-made irrigation water, the steaming of reduction soil moisture
Send out, so as to improve efficiency of water application.Water-loss reducer of soil can act also as soil conditioner, promote the formation of soil aggregate, from
And stable soil structure, reduce soil the ground temperature difference, improve permeability use.Simultaneously as inflatable after water-loss reducer of soil water suction
To hundreds and thousands of times of original volume, after water release, volume is bounced back again, so its expansion and contraction process, can change soil
The porousness of earth, can provide strong living environment for the activity of microorganism.Therefore, water-loss reducer of soil becomes raising moisture profit
With rate, the effective ways of increase crop yield.
Hydrogel is a more typical class soil water-retaining material, can form the water of three kinds of states, that is, tie inside and outside its structure
Heshui, irreducible water and Free water.Wherein Free water accounts for 98%, is effective water that crops are absorbable and utilize.But water
In acid or alkaline medium, its water absorbing capacity suddenly can be reduced gel, so as to affect which to acid or basic soil
Water retention property.Environmentally friendly water-loss reducer of soil meets environmental conservation and the requirement of social sustainable development, is that following soil is protected
The development trend of water preparation.But the existing material for preparing water-loss reducer of soil is mostly the derivant of petrochemicals, can not
Degraded by Soil Microorganism, thus the water conservation agent material of petroleum source can be retained in soil, cause environmental pollution etc. a series of
Problem.PH responsive types semi-interpenetrating network aqueous gel obtained by the present invention is degradable new material, therefore can meet the need for using
Ask.
The content of the invention
It is an object of the invention to overcome the defect of prior art, there is provided one kind prepares pH responsive type semi-intercrossing network water-settings
The preparation method of glue.PH sensitive hydrogel materials obtained in of the invention can keep larger suction in the range of pH 5~12
Outlet capacity, so as to the water-retaining agent of acidity or basic soil can be used it for.
The present invention's is achieved through the following technical solutions:
A kind of preparation method of pH responsive types semi-interpenetrating network aqueous gel, comprises the following steps:
Based on the mass fraction of raw material:
(1) 1 part of butt starch is placed in there-necked flask, adds 20 parts of distilled water, the gelatinizing 30min in 90 DEG C of water-baths
Afterwards, water-bath is dropped to into 60 DEG C;
(2) 2~6 parts of poly-aspartates are weighed, are dissolved in 4 parts of distilled water, it is agitated after obtain poly-aspartate
Solution, then 6 parts of acrylic acid are slowly dropped in poly-aspartate solution, poly-aspartate is obtained with acrylic acid mixture;
(3) poly-aspartate obtained by step (2) and acrylic acid mixture are added to into the starch obtained by step (1) slowly
In paste, after mixing 10min, 0.04 part of 0.1 part of initiator potassium persulfate and sodium sulfite, cross-linking agent di-2-ethylhexylphosphine oxide are sequentially added
0.04 part of acrylamide;
(4), after question response thing plastic, it is cut into 1cm3The blob of viscose of size, is placed in 5.0L tap waters and soaks 5 days, wash away
Unreacted starch, poly-aspartate, acrylic acid, two potassium sulfate of initiator and sodium sulfite, cross-linking agent methylene bisacrylamide acyl
After amine, sample is washed to neutrality, Jing air dry ovens are crushed in 80 DEG C of dryings to constant weight, pulverizer, cross 200 mesh sieves, obtain
PH sensitivity semi-interpenetrating network aqueous gels.
Preferably, in the step (2), poly-aspartate is 4 parts.The pH obtained by above-mentioned preparation method is sensitive
Type semi-interpenetrating network aqueous gel, its water absorbing capacity is presented water suction maximum at pH=6 and pH=11 in the range of the whole pH.
A kind of pH responsive types semi-interpenetrating network aqueous gel, follow these steps to prepare, and the raw material in terms of mass fraction is matched somebody with somebody
Than for:
(1) 1 part of butt starch is placed in there-necked flask, adds 20 parts of distilled water, the gelatinizing 30min in 90 DEG C of water-baths
Afterwards, water-bath is cooled to into 60 DEG C, obtains gelatinized corn starch;
(2) 2~6 parts of poly-aspartates are taken, are dissolved in 4 parts of distilled water, it is agitated after obtain poly-aspartate solution, then
6 parts of acrylic acid are slowly dropped in poly-aspartate solution, poly-aspartate are obtained with acrylic acid mixture;
(3) it is slow by the poly-aspartate obtained by step (2) and the acrylic acid mixture mixed starch for being added to step (1)
In paste, after mixing 10min, 0.1 part of initiator potassium persulfate, 0.04 part of sodium sulfite and cross-linking agent di-2-ethylhexylphosphine oxide are sequentially added
0.04 part of acrylamide;
(4), after question response thing plastic, it is cut into 1cm3Blob of viscose, be placed in 5.0L tap waters and soak 5d, wash away unreacted
Starch, poly-aspartate, acrylic acid, sodium sulfite, two potassium sulfate of initiator and sodium sulfite, cross-linking agent methylene bisacrylamide acyl
Amine, sample is washed to neutrality, is dried to constant weight, is crushed with pulverizer, cross 200 mesh sieves, obtain in 80 DEG C of air dry ovens
PH sensitivity semi-interpenetrating network aqueous gels.
Preferably, the poly-aspartate wherein in above-mentioned steps (2) is 4 parts.
Compared with prior art, the pH responsive types semi-interpenetrating network aqueous gel that prepared by the present invention has following significantly excellent
Point:
1st, in acid or alkaline medium, its water absorbing capacity suddenly can be reduced hydrogel, so as to reduce which to soil
Water retention property.PH sensitive hydrogels prepared by the present invention can keep larger water absorbing capacity in the range of pH 5~12
Power, so as to the water-retaining agent of acidity or basic soil can be used it for.
2nd, the monomer selected by existing synthesis water-loss reducer of soil can be left after petrochemical derivative, use mostly
In soil, soil yield is reduced, causes environmental pollution.In the present invention in prepared pH responsive type semi-interpenetrating network aqueous gels
Biodegradable starch and poly-aspartate are introduced, so as to the degradation rate of water-loss reducer of soil, therefore the present invention can be accelerated
In water-loss reducer of soil it is environmentally friendly.
Description of the drawings
Fig. 1:It is starch, polyacrylic acid, poly-aspartate and pH responsive type semi-intercrossing network water-settings in the embodiment of the present invention 1
The infrared spectrogram of glue.Description of reference numerals:From figure 1 it appears that pH responsive types semi-intercrossing network manufactured in the present embodiment
Possesses the characteristic absorption peak of starch, polyacrylic acid and poly-aspartate in hydrogel, such as in 1719cm-1Place occurs in that polyacrylic acid
- C=O stretching vibration peaks, in 1409cm-1、1560cm-1- C-N ,-C=in poly-aspartate lactams group is occurred in that respectively
The vibration peak of O keys, in 1021cm-1Place occurs in that the stretching vibration peak of-C-O-C on anhydroglucose ring in starch.
Fig. 2:It is that pH responsive types semi-interpenetrating network aqueous gel is inhaled in different pH value aqueous solutions in the embodiment of the present invention 1 to 3
The testing result of water-swellable multiplying power.Description of reference numerals, from figure 2 it can be seen that pH responsive type semi-interpenetrating network aqueous gels
Water absorption and swelling rate changes with the change of aqueous solution pH, and maximum swelling rate is not at pH=7, in the range of whole pH, molten
Swollen rate is presented bimodal, i.e. pH=6 and pH=11.
Fig. 3:It is the energy storage in pH=7 aqueous solutions in pH responsive type semi-interpenetrating network aqueous gels in the embodiment of the present invention 1 to 3
Modulus G ' with loss moduluses G " testing result.Description of reference numerals, from figure 3, it can be seen that sensitive with product pH is built
The rising of poly-aspartate content in type semi-interpenetrating network aqueous gel, its storage modulus G ' and loss moduluses G " it is presented what is reduced
Trend.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment, but embodiment of the present invention is not only limited
In this.Embodiment 1
(1) the butt common corn starch of 500g is placed in there-necked flask, adds the distilled water of 10L, in 90 DEG C of water-baths
In pot after gelatinizing 30min, water-bath is cooled to into 60 DEG C, gelatinized corn starch is obtained;
(2) 1000g poly-aspartates are weighed, is dissolved in 2L distilled water, after stirring, obtain poly-aspartate solution, after
And the acrylic acid of 3L is slowly dropped in poly-aspartate solution, poly-aspartate is obtained with acrylic acid mixture;
(3) poly-aspartate obtained by step (2) and acrylic acid mixture are added to into the shallow lake obtained by step (1) slowly
In paste mixing, after mixing 10min, initiator potassium persulfate 50g, sodium sulfite 20g and cross-linking agent di-2-ethylhexylphosphine oxide third are sequentially added
Acrylamide 20g;
(4), after question response thing plastic, it is cut into volume and is about 1cm3Blob of viscose (concrete size not limited to this), put
5d is soaked in 500L tap waters, after washing away unreacted starch, polyacrylic acid, poly-aspartate, initiator and cross-linking agent, will
Sample is washed to neutrality, in 80 DEG C of air dry oven dryings to constant weight, was crushed to 200 mesh sieves with pulverizer, and was obtained pH sensitive
Property semi-interpenetrating network aqueous gel finished product.
Water absorption of the pH responsive types semi-interpenetrating network aqueous gel manufactured in the present embodiment in pH=6, pH=7 and pH=11
Jing actual measurements are respectively 100.6g/mL, 95.6g/mL, 112.8g/mL.Starch, polyacrylic acid, poly-aspartate and pH responsive types half
Interpenetration network hydrogel infrared spectrogram is as shown in Figure 1.PH responsive types semi-interpenetrating network aqueous gel is in different pH value aqueous solutions
Water absorption and swelling multiplying power is as shown in Figure 2;PH responsive types semi-interpenetrating network aqueous gel storage moduluss G in pH=7 aqueous solutions ' and loss
Modulus G " is as shown in Figure 3.
Embodiment 2
(1) the butt common corn starch of 500g is placed in there-necked flask, adds the distilled water of 10L, in 90 DEG C of water-baths
In pot after gelatinizing 30min, water-bath is dropped to into 60 DEG C, gelatinized corn starch is obtained;
(2) 2000g poly-aspartates are weighed, is dissolved in 2L distilled water, after stirring, obtain poly-aspartate solution, after
And the acrylic acid of 3L is slowly dropped in poly-aspartate solution, poly-aspartate is obtained with acrylic acid mixture;
(3) poly-aspartate obtained by step (2) and acrylic acid mixture are added to into the starch obtained by step (1) slowly
In paste, after mixing 10min, initiator potassium persulfate 50g, sodium sulfite 20g are sequentially added;Cross-linking agent methylene bisacrylamide acyl
Amine 20g;
(4), after question response thing plastic, it is cut into volume and is about 1cm3Blob of viscose (blob of viscose size not limited to this), put
Soak 5 days in 500L tap waters, after washing away unreacted starch, polyacrylic acid, poly-aspartate, initiator and cross-linking agent,
Sample is washed to neutrality, in 80 DEG C of air dry oven dryings to constant weight, 200 mesh sieves was crushed to pulverizer, and was obtained pH quick
Perceptual semi-interpenetrating network aqueous gel finished product.
Water absorption of the pH responsive types semi-interpenetrating network aqueous gel manufactured in the present embodiment in pH=6, pH=7 and pH=11
Respectively 161.8g/mL, 152.4g/mL, 164.2g/mL.PH responsive types semi-interpenetrating network aqueous gel is in different pH value aqueous solutions
Middle water absorption and swelling multiplying power is as shown in Figure 2.PH responsive types semi-interpenetrating network aqueous gel storage moduluss G in pH=7 aqueous solutions ' and damage
Consumption modulus G " is as shown in Figure 3.
Embodiment 3
(1) the butt common corn starch of 500g is placed in there-necked flask, adds the distilled water of 10L, in 90 DEG C of water-baths
In pot after gelatinizing 30min, water-bath is dropped to into 60 DEG C, gelatinized corn starch is obtained;
(2) 3000g poly-aspartates are weighed, are dissolved in 2L distilled water, after stirring, are obtained poly-aspartate solution,
Then the acrylic acid of 3L is slowly dropped in poly-aspartate solution, poly-aspartate is obtained with acrylic acid mixture;
(3) poly-aspartate obtained by step (2) and acrylic acid mixture are added to into the starch obtained by step (1) slowly
In paste, after mixing 10min, initiator potassium persulfate 50g, sodium sulfite 20g, cross-linking agent methylene bisacrylamide acyl are sequentially added
Amine 20g;
(4), after question response thing plastic, it is cut into volume and is about 1cm3Blob of viscose (the concrete size not limited to this of blob of viscose), will
Which is placed in 5 00L tap waters and soaks 5 days, washes away unreacted starch, polyacrylic acid, poly-aspartate, initiator and crosslinking
After agent, sample is washed to neutrality, in 80 DEG C of air dry oven dryings to constant weight, 200 mesh sieves were crushed to pulverizer, and were obtained
PH sensitivity semi-interpenetrating network aqueous gel finished products.
The present embodiment prepares Water absorption Jing of the pH responsive types semi-interpenetrating network aqueous gel in pH=6, pH=7 and pH=11
Actual measurement is respectively 362.7g/mL, 362.1g/mL, 377.8g/mL.PH responsive types semi-interpenetrating network aqueous gel is in different pH value water
Water absorption and swelling multiplying power in solution is as shown in Fig. 2 pH responsive types semi-interpenetrating network aqueous gel storage moduluss G in pH=7 aqueous solutions '
With loss moduluses G " as shown in Figure 3.
Claims (4)
1. a kind of preparation method of pH responsive types semi-interpenetrating network aqueous gel, it is characterised in that comprise the following steps, with mass parts
The proportioning raw materials of number meter are as follows:
(1) 1 part of butt starch is placed in there-necked flask, adds 20 parts of distilled water, after gelatinizing 30min in 90 DEG C of water-baths,
Water-bath pot temperature is down to into 60 DEG C, gelatinized corn starch is obtained;
(2) 2~6 parts of poly-aspartates are taken, are dissolved in 4 parts of distilled water, it is agitated after poly-aspartate solution, then by 6 parts
Acrylic acid is slowly dropped in poly-aspartate solution, obtains poly-aspartate with acrylic acid mixture;
(3) poly-aspartate obtained by step (2) and acrylic acid mixture are added to into the gelatinized corn starch obtained by step (1) slowly
In, after mixing 10min, sequentially add 0.1 part of initiator potassium persulfate, 0.04 part of sodium sulfite, cross-linking agent di-2-ethylhexylphosphine oxide third
0.04 part of acrylamide;
(4), after question response thing plastic, it is cut into 1cm3Blob of viscose, be placed in 5.0L tap waters and soak 5d, wash away unreacted starch,
Poly-aspartate, acrylic acid, two potassium sulfate of initiator and sodium sulfite, after cross-linking agent bisacrylamide, sample are washed
To neutral, it is dried to constant weight in 80 DEG C of air dry ovens, is crushed with pulverizer, cross 200 mesh sieves, obtain pH sensitivity Semi-IPN
Network aqueous gel.
2. a kind of preparation method of pH responsive types semi-interpenetrating network aqueous gel according to claim 1, it is characterised in that step
Suddenly the poly-aspartate in (2) is 4 parts.
3. a kind of pH responsive types semi-interpenetrating network aqueous gel, it is characterised in that follow these steps to prepare, in terms of mass fraction
Proportioning raw materials meter:
(1) 1 part of butt starch is placed in there-necked flask, adds 20 parts of distilled water, after gelatinizing 30min in 90 DEG C of water-baths,
Water-bath is cooled to into 60 DEG C, gelatinized corn starch is obtained;
(2) 2~6 parts of poly-aspartates are taken, are dissolved in 4 parts of distilled water, it is agitated after obtain poly-aspartate solution, then by 6
Part acrylic acid is slowly dropped in poly-aspartate solution, obtains poly-aspartate with acrylic acid mixture;
(3) it is slow by the poly-aspartate obtained by step (2) and the acrylic acid mixture mixed gelatinized corn starch for being added to step (1)
In, after mixing 10min, sequentially add 0.1 part of initiator potassium persulfate, 0.04 part of sodium sulfite and cross-linking agent di-2-ethylhexylphosphine oxide third
0.04 part of acrylamide;
(4), after question response thing plastic, it is cut into 1cm3Blob of viscose, be placed in 5.0L tap waters and soak 5d, wash away unreacted starch,
Poly-aspartate, acrylic acid, sodium sulfite, two potassium sulfate of initiator and sodium sulfite, cross-linking agent methylene-bisacrylamide will
Sample is washed to neutrality, is dried to constant weight, is crushed with pulverizer, cross 200 mesh sieves, obtain pH sensitive in 80 DEG C of air dry ovens
Property semi-interpenetrating network aqueous gel.
4. a kind of pH responsive types semi-interpenetrating network aqueous gel as claimed in claim 3, it is characterised in that poly- in step (2)
Aspartic acid is 4 parts.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108484936A (en) * | 2018-03-29 | 2018-09-04 | 广州迈普再生医学科技股份有限公司 | A kind of hydrogel and its preparation method and application prepared by graft modification material |
CN114058022A (en) * | 2021-12-21 | 2022-02-18 | 郑州沃尔德农业科技有限公司 | Amino acid slow-release fertilizer water-retaining agent, preparation method and application method |
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CN102690399A (en) * | 2012-06-14 | 2012-09-26 | 太原理工大学 | Polyaspartate/polyacrylic acid copolymer IPN (Interpenetrating Polymer Networks) hydrogel and preparation method thereof |
CN104327208A (en) * | 2014-10-28 | 2015-02-04 | 太原理工大学 | Preparation method of polyaspartic acid/ polyacrylic acid interpenetrating network super absorbent resin |
CN105232467A (en) * | 2015-10-26 | 2016-01-13 | 郑杉水 | Polyacrylamide gel peptization instant solid composite and preparing method thereof |
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CN102690399A (en) * | 2012-06-14 | 2012-09-26 | 太原理工大学 | Polyaspartate/polyacrylic acid copolymer IPN (Interpenetrating Polymer Networks) hydrogel and preparation method thereof |
CN104327208A (en) * | 2014-10-28 | 2015-02-04 | 太原理工大学 | Preparation method of polyaspartic acid/ polyacrylic acid interpenetrating network super absorbent resin |
CN105232467A (en) * | 2015-10-26 | 2016-01-13 | 郑杉水 | Polyacrylamide gel peptization instant solid composite and preparing method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108484936A (en) * | 2018-03-29 | 2018-09-04 | 广州迈普再生医学科技股份有限公司 | A kind of hydrogel and its preparation method and application prepared by graft modification material |
CN108484936B (en) * | 2018-03-29 | 2020-12-29 | 广州迈普再生医学科技股份有限公司 | Hydrogel prepared from graft modified material and preparation method and application thereof |
CN114058022A (en) * | 2021-12-21 | 2022-02-18 | 郑州沃尔德农业科技有限公司 | Amino acid slow-release fertilizer water-retaining agent, preparation method and application method |
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