CN108675674A - A kind of Novel dry powder mortar water-retaining agent and preparation method thereof - Google Patents
A kind of Novel dry powder mortar water-retaining agent and preparation method thereof Download PDFInfo
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- CN108675674A CN108675674A CN201810373330.3A CN201810373330A CN108675674A CN 108675674 A CN108675674 A CN 108675674A CN 201810373330 A CN201810373330 A CN 201810373330A CN 108675674 A CN108675674 A CN 108675674A
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- dry powder
- retaining agent
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/38—Polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/46—Water-loss or fluid-loss reducers, hygroscopic or hydrophilic agents, water retention agents
- C04B2103/465—Water-sorbing agents, hygroscopic or hydrophilic agents
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- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Structural Engineering (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention belongs to building dry powder mortar additive technology fields, and in particular to a kind of Novel dry powder mortar water-retaining agent and preparation method thereof, the preparation method includes:(1) crosslinking agent is added into starch solution, heats up in atmosphere of inert gases, stirs isothermal holding, cooling is spare;(2) sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate are sequentially added into step (1), stirred in atmosphere of inert gases and is warming up to 55 DEG C, holding 200min;(3) absolute ethyl alcohol that 2 times of volumes are added is precipitated, and is filtered and is washed with absolute ethyl alcohol, is then dried in vacuo;(4) put into Universalpulverizer in crush powder to get the water-retaining agent;The present invention passes through acrylic acid modified Starch formation starch ether, then the 3 D stereo reticular structure with more hydrophilic radical is formed by crosslinking agent, multiple hydrones are firmly adsorbed by the hydrogen bond action between the multiple hydroxyls and hydrone on the mesh carrier of modified starch ether, it is ensured that its water retention property.
Description
Technical field
The invention belongs to building dry powder mortar additive technology fields, and in particular to a kind of Novel dry powder mortar water-retaining agent
And preparation method thereof.
Background technology
Dry powder and mortar refers to aggregate (such as quartz sand), inorganic coagulation material (such as cement) and addition through dry screening process
Agent (such as polymer) etc. carries out a kind of graininess or powdery made of physical mixed by a certain percentage, in the form of packed or is in bulk
It is transported to building site, the material that can be used directly after adding water to mix and stir.Also referred to as dry mortar powder, dry blend, dry mixing powder, some buildings
Binder also belongs to such.Dry powder and mortar plays bonding, liner, protection and decoration function, application in building trade with thin layer
Extremely extensively.
Dry powder and mortar uses water-retaining agent as the typical additives of dry powder and mortar, has to the raising of its water retention property very heavy
The effect wanted.In the prior art, the raw material of dry powder and mortar water-retaining agent includes mainly:Organic (cellulose ether and starch ether) and
Inorganic (high adsorption silicate mineral);Cellulose ether has excellent water retention property, is widely used in dry powder and mortar guarantor
In aqua, but as the price of timber and cotton rises steadily, the price of cellulose ether also remains high, it usually needs 20,000
Yuan/ton so that the cost of dry powder and mortar water-retaining agent greatly improves;High adsorption silicate mineral is although cheap, still
The gap of water retention property and organic water-retaining agent is still very big, it is difficult to meet the requirement of existing dry powder and mortar water retention property.
Invention content
For the problems of the prior art, the purpose of the present invention is to provide a kind of systems of Novel dry powder mortar water-retaining agent
Preparation Method reduces the manufacturing cost of dry powder and mortar water-retaining agent;The dry powder and mortar water-retaining agent being prepared has excellent water conservation
Performance.
To achieve the goals above, the present invention is achieved by the following scheme:
A kind of preparation method of Novel dry powder mortar water-retaining agent, includes the following steps:
(1) crosslinking agent is added into starch solution, 85 DEG C are warming up in atmosphere of inert gases, stirs isothermal holding
30min is then cooled down spare;
(2) sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate are sequentially added into the reaction system of step (1), in inertia
It is stirred in atmosphere, is then warming up to 55 DEG C, and keep 200min;
(3) absolute ethyl alcohol that 2 times of volumes are added into the reaction system of step (2) is precipitated, and is filtered and with anhydrous
Ethyl alcohol washing precipitation 2~3 times, is then dried in vacuo precipitation at a temperature of 60 DEG C;
(4) will crush in the precipitation input Universalpulverizer of step (3) powder to get the described dry powder and mortar water conservation
Agent.
Preferably, the crosslinking agent is selected from crown ether, beta-cyclodextrin, N, one kind in N '-methylene-bisacrylamides.
Preferably, in step (1), after the completion of reaction, cooling treatment is carried out to reaction system using ice-water bath.
Preferably, in step (2), the mass ratio of the sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate is 1:
(0.010~0.013):(0.011~0.014).
Preferably, in step (2), the warming temperature of mixed system is set as 50 DEG C, the temperature of system to be mixed is stablized
It is 55 DEG C that warming temperature is arranged again after 50 DEG C.
The present invention also provides a kind of Novel dry powder mortar water-retaining agent being prepared such as above-mentioned preparation method.
In the present invention, by acrylic acid modified Starch formation starch ether, then formed with more hydrophilic by crosslinking agent
The 3 D stereo reticular structure of group is made by the hydrogen bond between the multiple hydroxyls and hydrone on the mesh carrier of modified starch ether
With can firmly adsorb multiple hydrones;Meanwhile then side-chain bulk also accordingly increases for the increase of molecular weight, the grid effect of formation
Should be also all the more apparent, therefore further improve its water retention property.
The product that the present invention is prepared has good biodegradable properties, also have excellent water retention property and compared with
Low cost.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is furture elucidated.
In order to further improve the water holding capacity of dry powder and mortar water-retaining agent, the cost of water-retaining agent is reduced, the present invention carries
For a kind of preparation method of Novel dry powder mortar water-retaining agent, include the following steps:
(1) crosslinking agent is added into starch solution, 85 DEG C are warming up in atmosphere of inert gases, stirs isothermal holding
30min is then cooled down spare;
(2) sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate are sequentially added into the reaction system of step (1), in inertia
It is stirred in atmosphere, is then warming up to 55 DEG C, and keep 200min;
(3) absolute ethyl alcohol that 2 times of volumes are added into the reaction system of step (2) is precipitated, and is filtered and with anhydrous
Ethyl alcohol washing precipitation 2~3 times, is then dried in vacuo precipitation at a temperature of 60 DEG C;
(4) will crush in the precipitation input Universalpulverizer of step (3) powder to get the described dry powder and mortar water conservation
Agent.
In the present invention, processing is modified to starch by acrylic acid and forms starch ether, then under the action of crosslinking agent
Being formed has the 3 D stereo reticular structure of more hydrophilic radical, multiple hydroxyls and water on the mesh carrier by modified starch ether
Intermolecular hydrogen bond action can securely adsorb multiple hydrones, so that it is guaranteed that the water-retaining agent has excellent water holding capacity;This
Outside, then side-chain bulk is also bigger for molecular weight increase, grid effect is formed by also all the more obviously, to further ensure its tool
There is good water-retaining property.
The present invention is using starch as bulk, and with excellent biodegradable properties, manufacturing cost is lower.
According to the present invention, starch of the present invention, can select it is familiar to those skilled in the art, specifically, can
To enumerate one kind or combinations thereof in cornstarch, tapioca, wheaten starch, sweet potato starch and guar gum.
In the present invention, the effect of crosslinking agent is that the starch ether after modification forms 3 D stereo reticular structure, described
Crosslinking agent can select Physical crosslinking agent or chemical cross-linking agent, specifically, the Physical crosslinking agent can enumerate crown ether and
Beta-cyclodextrin, the chemical cross-linking agent can enumerate N, N '-methylene-bisacrylamides, preferably, institute in the present invention
The crosslinking agent stated is preferably Physical crosslinking agent, particularly preferred crown ether.
In the present invention, in order to improve the cooling efficiency of reaction system in step (1), after completion of the reaction, using ice-water bath
Cooling treatment is carried out to reaction system.
In the present invention, the additive amount of the sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate can be in a wider scope
Selection, preferably, the mass ratio of the sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate is 1:(0.010~
0.013):(0.011~0.014).
In the present invention, in step (2), the warming temperature of mixed system is set as 50 DEG C, the temperature of system to be mixed
It is 55 DEG C to stablize and warming temperature is arranged again after 50 DEG C;It was found by the inventors of the present invention that must have after temperature is increased to 50 DEG C slow
Punching, such setting can be too fast to avoid the polymerization speed caused by temperature is excessively high, improves the stability of reaction system.
The present invention also provides a kind of Novel dry powder mortar water-retaining agent being prepared using above-mentioned preparation method.
Below by way of the technological merit of the specific embodiment present invention further elucidated above.
Embodiment 1
A kind of preparation method of Novel dry powder mortar water-retaining agent, includes the following steps:
(1) 5.006g guar gums, 0.255g beta-cyclodextrins are added in 250mL three-necked flasks, 100mL is then added
Distilled water, stirring, 30min is kept the temperature after being warming up to 85 DEG C, a straight-through nitrogen protection during being somebody's turn to do;Then it will be gelatinized at room temperature
Starch cool, can also use ice-water bath accelerate cooling procedure;
(2) 27mL distilled water is measured, is positioned in 100mL beakers, is weighed 4.126g sodium hydroxides and be put into the beaker, gently
It shakes beaker to be completely dissolved by sodium hydroxide, which is positioned in draught cupboard and is cooled down;
11.8mL acrylic acid is measured with measuring cup, is positioned in 100mL beakers, sodium hydroxide solution after cooling is being stirred
Under be added slowly in acrylic acid, control, which is added speed and not release a large amount of thermal conductivities, causes acrylic acid auto polymerizations, will after addition
The mixture is cooled to room temperature for use;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.110g sodium hydrogensulfites and be put into the beaker, jog
Beaker is completely dissolved by it;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.115g potassium peroxydisulfates and be put into the beaker, with stirring
Stick stirring allows it to be completely dissolved;
Sodium acrylate solution, solution of sodium bisulfite, potassium persulfate solution are poured into the reactant being cooled to room temperature successively
In system, continues to stir 30min to being uniformly mixed, nitrogen protection is led in whole process;
It is warming up to 55 DEG C and keeps 200min.Can temperature be first set in 50 DEG C when heating, wait for that temperature is stablized at 50 DEG C
When temperature is adjusted to 55 DEG C again;
(3) viscous fluid after reaction is poured into 1000mL beakers, the absolute ethyl alcohol for being added with stirring 2 times of volumes is sunk
It forms sediment, has white sticky Precipitation at this time, utilize absolute ethyl alcohol to wash 3 times again after filtering, obtain white solid sample;By sample
Product are shredded with scissors, are dried in vacuo for 24 hours at 60 DEG C;
(4) the Universalpulverizer high speed of the sample after drying is crushed into 1min, obtains white powder, is sealed after taking-up,
Up to the Novel dry powder mortar water-retaining agent.
Embodiment 2
A kind of preparation method of Novel dry powder mortar water-retaining agent, includes the following steps:
(1) 5.046g guar gums, 0.26g crown ethers are added in 250mL three-necked flasks, 100mL distillations is then added
Water, stirring, 30min is kept the temperature after being warming up to 85 DEG C, a straight-through nitrogen protection during being somebody's turn to do;Then the shallow lake that will be gelatinized at room temperature
Powder cools down, and can also accelerate cooling procedure with ice-water bath;
(2) 27mL distilled water is measured, is positioned in 100mL beakers, is weighed 4.126g sodium hydroxides and be put into the beaker, gently
It shakes beaker to be completely dissolved by sodium hydroxide, which is positioned in draught cupboard and is cooled down;
11.8mL acrylic acid is measured with measuring cup, is positioned in 100mL beakers, sodium hydroxide solution after cooling is being stirred
Under be added slowly in acrylic acid, control, which is added speed and not release a large amount of thermal conductivities, causes acrylic acid auto polymerizations, will after addition
The mixture is cooled to room temperature for use;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.110g sodium hydrogensulfites and be put into the beaker, jog
Beaker is completely dissolved by it;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.115g potassium peroxydisulfates and be put into the beaker, with stirring
Stick stirring allows it to be completely dissolved;
Sodium acrylate solution, solution of sodium bisulfite, potassium persulfate solution are poured into the reactant being cooled to room temperature successively
In system, continues to stir 30min to being uniformly mixed, nitrogen protection is led in whole process;
It is warming up to 55 DEG C and keeps 200min.Can temperature be first set in 50 DEG C when heating, wait for that temperature is stablized at 50 DEG C
When temperature is adjusted to 55 DEG C again;
(3) viscous fluid after reaction is poured into 1000mL beakers, the absolute ethyl alcohol for being added with stirring 2 times of volumes is sunk
It forms sediment, has white sticky Precipitation at this time, utilize absolute ethyl alcohol to wash 3 times again after filtering, obtain white solid sample;By sample
Product are shredded with scissors, are dried in vacuo for 24 hours at 60 DEG C;
(4) the Universalpulverizer high speed of the sample after drying is crushed into 1min, obtains white powder, is sealed after taking-up,
Up to the Novel dry powder mortar water-retaining agent.
Embodiment 3
A kind of preparation method of Novel dry powder mortar water-retaining agent, includes the following steps:
(1) 5.072g cornstarch, 0.253g crown ethers are added in 250mL three-necked flasks, 100mL distillations is then added
Water, stirring, 30min is kept the temperature after being warming up to 85 DEG C, a straight-through nitrogen protection during being somebody's turn to do;Then the shallow lake that will be gelatinized at room temperature
Powder cools down, and can also accelerate cooling procedure with ice-water bath;
(2) 27mL distilled water is measured, is positioned in 100mL beakers, is weighed 4.126g sodium hydroxides and be put into the beaker, gently
It shakes beaker to be completely dissolved by sodium hydroxide, which is positioned in draught cupboard and is cooled down;
11.8mL acrylic acid is measured with measuring cup, is positioned in 100mL beakers, sodium hydroxide solution after cooling is being stirred
Under be added slowly in acrylic acid, control, which is added speed and not release a large amount of thermal conductivities, causes acrylic acid auto polymerizations, will after addition
The mixture is cooled to room temperature for use;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.110g sodium hydrogensulfites and be put into the beaker, jog
Beaker is completely dissolved by it;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.115g potassium peroxydisulfates and be put into the beaker, with stirring
Stick stirring allows it to be completely dissolved;
Sodium acrylate solution, solution of sodium bisulfite, potassium persulfate solution are poured into the reactant being cooled to room temperature successively
In system, continues to stir 30min to being uniformly mixed, nitrogen protection is led in whole process;
It is warming up to 55 DEG C and keeps 200min.Can temperature be first set in 50 DEG C when heating, wait for that temperature is stablized at 50 DEG C
When temperature is adjusted to 55 DEG C again;
(3) viscous fluid after reaction is poured into 1000mL beakers, the absolute ethyl alcohol for being added with stirring 2 times of volumes is sunk
It forms sediment, has white sticky Precipitation at this time, utilize absolute ethyl alcohol to wash 3 times again after filtering, obtain white solid sample;By sample
Product are shredded with scissors, are dried in vacuo for 24 hours at 60 DEG C;
(4) the Universalpulverizer high speed of the sample after drying is crushed into 1min, obtains white powder, is sealed after taking-up,
Up to the Novel dry powder mortar water-retaining agent.
Embodiment 4
A kind of preparation method of Novel dry powder mortar water-retaining agent, includes the following steps:
(1) 5.013g cornstarch, 0.257g beta-cyclodextrins are added in 250mL three-necked flasks, 100mL is then added
Distilled water, stirring, 30min is kept the temperature after being warming up to 85 DEG C, a straight-through nitrogen protection during being somebody's turn to do;Then it will be gelatinized at room temperature
Starch cool, can also use ice-water bath accelerate cooling procedure;
(2) 27mL distilled water is measured, is positioned in 100mL beakers, is weighed 4.161g sodium hydroxides and be put into the beaker, gently
It shakes beaker to be completely dissolved by sodium hydroxide, which is positioned in draught cupboard and is cooled down;
11.8mL acrylic acid is measured with measuring cup, is positioned in 100mL beakers, sodium hydroxide solution after cooling is being stirred
Under be added slowly in acrylic acid, control, which is added speed and not release a large amount of thermal conductivities, causes acrylic acid auto polymerizations, will after addition
The mixture is cooled to room temperature for use;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.102g sodium hydrogensulfites and be put into the beaker, jog
Beaker is completely dissolved by it;
10mL distilled water is measured, is positioned in 50mL beakers, is weighed 0.109g potassium peroxydisulfates and be put into the beaker, with stirring
Stick stirring allows it to be completely dissolved;
Sodium acrylate solution, solution of sodium bisulfite, potassium persulfate solution are poured into the reactant being cooled to room temperature successively
In system, continues to stir 30min to being uniformly mixed, nitrogen protection is led in whole process;
It is warming up to 55 DEG C and keeps 200min.Can temperature be first set in 50 DEG C when heating, wait for that temperature is stablized at 50 DEG C
When temperature is adjusted to 55 DEG C again;
(3) viscous fluid after reaction is poured into 1000mL beakers, the absolute ethyl alcohol for being added with stirring 2 times of volumes is sunk
It forms sediment, has white sticky Precipitation at this time, utilize absolute ethyl alcohol to wash 3 times again after filtering, obtain white solid sample;By sample
Product are shredded with scissors, are dried in vacuo for 24 hours at 60 DEG C;
(4) the Universalpulverizer high speed of the sample after drying is crushed into 1min, obtains white powder, is sealed after taking-up,
Up to the Novel dry powder mortar water-retaining agent.
It is carried out by sand aerated concrete block wall application technology regulation Appendix B water retention test method (DBJ/CT035)
Water retention test, water retention are water-retaining property of the fresh mortar after filter paper absorbs water 15 minutes.
Test items refer to after the water-retaining agent 2g that 500g cement, 500g fine sands and above-described embodiment 1-4 are prepared is mixed
Mark;
As a control group with the general fibre element ethers water-retaining agent bought in the market, other conditions are constant, carry out comparison survey
Examination, specific test data are shown in Table 1.
Table 1:
Water-retaining property/(mg/cm2) | Consistency/mm | Bleeding rate/% | Compression strength/Mpa | |
Embodiment 1 | 7.9 | 49 | 0.15 | 27.8 |
Embodiment 2 | 7.5 | 49 | 0.16 | 27.6 |
Embodiment 3 | 7.3 | 49 | 0.15 | 27.8 |
Embodiment 4 | 7.4 | 48 | 0.15 | 27.4 |
Control group | 5.1 | 49 | 0.15 | 26.5 |
In conjunction with above-mentioned test data, Novel dry powder mortar provided by the invention has excellent water retention property with water-retaining agent.
The basic principles and main features and the features of the present invention of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement is both fallen in the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (6)
1. a kind of preparation method of Novel dry powder mortar water-retaining agent, it is characterised in that:Include the following steps:
(1) crosslinking agent is added into starch solution, 85 DEG C are warming up in atmosphere of inert gases, stirs isothermal holding 30min, connects
It is spare cooling;
(2) sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate are sequentially added into the reaction system of step (1), in inert gas
It is stirred in atmosphere, is then warming up to 55 DEG C, and keep 200min;
(3) absolute ethyl alcohol that 2 times of volumes are added into the reaction system of step (2) is precipitated, and is filtered and is used absolute ethyl alcohol
Washing precipitation 2~3 times, is then dried in vacuo precipitation at a temperature of 60 DEG C;
(4) will the precipitation of step (3) put into Universalpulverizer in crush powder to get the dry powder and mortar water-retaining agent.
2. the preparation method of Novel dry powder mortar water-retaining agent according to claim 1, it is characterised in that:The crosslinking
Agent is selected from crown ether, beta-cyclodextrin, N, one kind in N '-methylene-bisacrylamides.
3. the preparation method of Novel dry powder mortar water-retaining agent according to claim 1, it is characterised in that:In step (1),
After the completion of reaction, cooling treatment is carried out to reaction system using ice-water bath.
4. the preparation method of Novel dry powder mortar water-retaining agent according to claim 1, it is characterised in that:In step (2),
The mass ratio of the sodium acrylate, sodium hydrogensulfite and potassium peroxydisulfate is 1:(0.010~0.013):(0.011~0.014).
5. the preparation method of Novel dry powder mortar water-retaining agent according to claim 1, it is characterised in that:In step (2),
The warming temperature of mixed system is set as 50 DEG C, it is 55 that warming temperature, which is arranged, in the temperature stabilization of system to be mixed again after 50 DEG C
℃。
6. a kind of Novel dry powder mortar water-retaining agent that preparation method as claimed in any one of claims 1 to 5, wherein is prepared.
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CN102060959A (en) * | 2010-12-03 | 2011-05-18 | 中国科学院长春应用化学研究所 | Method for preparing polyacrylic acid water-retaining agent |
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CN103333291A (en) * | 2013-07-11 | 2013-10-02 | 合肥工业大学 | Preparation method of starch water-retaining agent with high gel strength |
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