CN105461844A - Preparation method for composite resin - Google Patents
Preparation method for composite resin Download PDFInfo
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- CN105461844A CN105461844A CN201410435788.9A CN201410435788A CN105461844A CN 105461844 A CN105461844 A CN 105461844A CN 201410435788 A CN201410435788 A CN 201410435788A CN 105461844 A CN105461844 A CN 105461844A
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Abstract
The invention relates to a preparation method for composite resin and belongs to the technical field of preparation methods for resin, and particularly relates to a preparation method for composite resin. The invention provides the preparation method for composite resin, wherein the water-absorbing property of the composite resin is good and the rigidity thereof is good. The preparation method comprises the following steps: 1) weighing a certain amount of a methacrylic acid monomer, neutralizing the monomer with potassium hydroxide, mixing the the obtained product with intercalation modified kaolin, and stirring the mixture to make potassium methacrylate enter interlayers to prepare a monomer solution; 2) weighing a certain amount of potassium persulfate and N,N-methylene bisacrylamide, pouring potassium persulfate and N,N-methylene bisacrylamide into a flask with cyclohexane with a certain volume, adding a dispersant, fully stirring the mixture, then adding the prepared monomer solution, raising the temperature such that a crosslinking copolymerization reaction is quickly conducted among interlayers of kaolin; and 3) performing suction filtration on the mixture in the flask, washing the obtained material with anhydrous ethanol for three times, and carrying out drying the mixture; and in addition, preparing polypotassium methacrylate without kaolin for comparison; and determining the water-absorbing rate, the water-retaining capacity and the strength of resin absorbing water.
Description
Technical field
The invention belongs to preparation method's technical field of resin, particularly relate to a kind of preparation method of compound resin.
Background technology
The compound of polymkeric substance and clay is the important component part of nanometer science and technology, is also one of important method preparing high-performance polymer material.Super water absorbent resin is a kind of new function high molecular polymer, it is structurally lightly crosslinked three-dimensional space net structure, containing many hydrophilic radicals, can specific absorption own wt heavy the hundred times even water of several thousand times, water retention property is good, even if when pressurize also not dehydration or dehydration little, the aspects such as agricultural gardening, food, medical and health, civil construction, petrochemical complex are widely used in, but also there are some weakness at present in super water absorbent resin, as water-retaining capacity not easily improves, rigidity and plasticity-are general lower.
Summary of the invention
The present invention is exactly for the problems referred to above, provides the preparation method of the compound resin of a kind of good water absorption, good rigidly.
For achieving the above object, the present invention includes following steps.
1) take a certain amount of monomer-methacrylic acid, with potassium hydroxide neutralization, mix with the kaolin after intercalation modifying, stir, make-methacrylic acid potassium enters interlayer, obtains monomer solution.
2) a certain amount of Potassium Persulphate and N, N is taken '-methylene-bisacrylamide, in the flask of hexanaphthene entering to be equipped with certain volume, add dispersion agent, add the monomer solution configured after abundant stirring, heat up, copolymerzation with cross-linking reaction occurs rapidly at kaolin interlayer.
3) by mixture suction filtration in flask, with absolute ethanol washing three times, dry; In addition, preparation does not add kaolinic polymethyl acrylic acid potassium resin, for contrast; Measure mechanical strength of resin after its rate of water absorption, water retention capacity and water suction.
4) the resin centrifugation will fully absorbed water, weighs centrifugal front and back resin quality.
5) get quantitative resin, be laid in glass dish after complete swelling, slide glass is placed on gel, record slide glass upper limb height with hypsograph, take reading
l1, then counterweight is placed on slide glass, the height of record slide glass upper limb
l2, average.
As a kind of preferred version, the present invention 1) take a certain amount of monomer-methacrylic acid, neutralize with potassium hydroxide, pH is adjusted in 6.8 ~ 7.2 scopes, mixes with the kaolin after intercalation modifying, at 50 DEG C, stir 3h, make-methacrylic acid potassium enters interlayer, obtained monomer solution.
2) a certain amount of Potassium Persulphate and N, N is taken '-methylene-bisacrylamide, in the flask of hexanaphthene entering to be equipped with certain volume, add dispersion agent, add the monomer solution configured after abundant stirring, be warming up to 60 DEG C, copolymerzation with cross-linking reaction occurs rapidly at kaolin interlayer.
As another kind of preferred version, the present invention 5) get quantitative resin, be laid in glass dish after complete swelling, slide glass be placed on gel, record slide glass upper limb height with hypsograph, take reading
l1, then 20g counterweight is placed on slide glass, the height of slide glass upper limb is recorded every 10s
l2, in triplicate, average.
Beneficial effect of the present invention.
The space that can provide after the methacrylic acid potassium monomer space entered required for kaolin interlayer of the present invention is less than Potassium ethanoate intercalation, illustrates that Potassium ethanoate is a kind of suitable intercalator in this experiment.But monomer does not replace Potassium ethanoate completely, reason may be this substitution reaction is a kind of reversible reaction, and reaction proceeds to a certain degree just reach balance.If improve the degree that substitution reaction is carried out, can attempt suitably increasing temperature of reaction and monomer consumption.Kaolinicly add the water absorbing properties substantially improving absorbent resin.
Embodiment
The present invention includes following steps.
1) take a certain amount of monomer-methacrylic acid, with potassium hydroxide neutralization, mix with the kaolin after intercalation modifying, stir, make-methacrylic acid potassium enters interlayer, obtains monomer solution.
2) a certain amount of Potassium Persulphate and N, N is taken '-methylene-bisacrylamide, in the flask of hexanaphthene entering to be equipped with certain volume, add dispersion agent, add the monomer solution configured after abundant stirring, heat up, copolymerzation with cross-linking reaction occurs rapidly at kaolin interlayer.
3) by mixture suction filtration in flask, with absolute ethanol washing three times, dry; In addition, preparation does not add kaolinic polymethyl acrylic acid potassium resin, for contrast; Measure mechanical strength of resin after its rate of water absorption, water retention capacity and water suction.
4) the resin centrifugation will fully absorbed water, weighs centrifugal front and back resin quality.
5) get quantitative resin, be laid in glass dish after complete swelling, slide glass is placed on gel, record slide glass upper limb height with hypsograph, take reading
l1, then counterweight is placed on slide glass, the height of record slide glass upper limb
l2, average.
The present invention 1) take a certain amount of monomer-methacrylic acid, with potassium hydroxide neutralization, pH is adjusted in 6.8 ~ 7.2 scopes, mix with the kaolin after intercalation modifying, at 50 DEG C, stir 3h, make-methacrylic acid potassium enters interlayer, obtains monomer solution.
2) a certain amount of Potassium Persulphate and N, N is taken '-methylene-bisacrylamide, in the flask of hexanaphthene entering to be equipped with certain volume, add dispersion agent, add the monomer solution configured after abundant stirring, be warming up to 60 DEG C, copolymerzation with cross-linking reaction occurs rapidly at kaolin interlayer.
The present invention 5) get quantitative resin, be laid in glass dish after complete swelling, slide glass be placed on gel, record slide glass upper limb height with hypsograph, take reading
l1, then 20g counterweight is placed on slide glass, the height of slide glass upper limb is recorded every 10s
l2, in triplicate, average.
Clay mineral as nano composite material presoma generally has laminate structure, and interfloor distance size is all at nano level.Interlayer often has activity, makes some organic molecule, polymkeric substance (or monomer) can insert the interlayer of main body as object, thus forms clay/organic nano level intercalated compound.Kaolin is as one of the widest clay mineral of distributed in nature, many excellent properties of its organic intercalation composition progressively become the focus infusion method that material scholars pay close attention to and move to left to 1.4244nm place through the kaolin d001 value that Potassium ethanoate is modified, very strong diffraction peak is there is at 1.4244nm place, at 0.7249nm place, former diffraction peak intensity reduces greatly, this illustrates that its interlamellar spacing increases greatly than the interlamellar spacing of protokaolin, Potassium ethanoate enters kaolin interlayer, and intercalation effect is obvious.
The diffraction peak intensity soaking the 1.4244nm place that graft process obtains is very weak, intercalation rate is low, intercalation effect is bad, because kaolin inter-layer bonding force is larger, realizing intercalation must by powerful external force as grinding or violent mechanical stirring, and moving by means of only molecular diffusion is be difficult to reach good intercalation effect.Have a large amount of methacrylic acid potassium to replace Potassium ethanoate and insert kaolin interlayer, interlamellar spacing is 1.167nm.
Above content be the present invention is done in conjunction with concrete preferred implementation further description, can not assert that specific embodiment of the invention is confined to these and illustrates, for general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to the protection domain that claims that the present invention submits to determine.
Claims (3)
1. a preparation method for compound resin, is characterized in that comprising the following steps:
1) take a certain amount of monomer-methacrylic acid, with potassium hydroxide neutralization, mix with the kaolin after intercalation modifying, stir, make-methacrylic acid potassium enters interlayer, obtains monomer solution;
2) a certain amount of Potassium Persulphate and N, N is taken '-methylene-bisacrylamide, in the flask of hexanaphthene entering to be equipped with certain volume, add dispersion agent, add the monomer solution configured after abundant stirring, heat up, copolymerzation with cross-linking reaction occurs rapidly at kaolin interlayer;
3) by mixture suction filtration in flask, with absolute ethanol washing three times, dry; In addition, preparation does not add kaolinic polymethyl acrylic acid potassium resin, for contrast; Measure mechanical strength of resin after its rate of water absorption, water retention capacity and water suction;
4) the resin centrifugation will fully absorbed water, weighs centrifugal front and back resin quality;
5) get quantitative resin, be laid in glass dish after complete swelling, slide glass is placed on gel, record slide glass upper limb height with hypsograph, take reading
l1, then counterweight is placed on slide glass, the height of record slide glass upper limb
l2, average.
2. the preparation method of a kind of compound resin according to claim 1, it is characterized in that 1) take a certain amount of monomer-methacrylic acid, neutralize with potassium hydroxide, pH is adjusted in 6.8 ~ 7.2 scopes, mix with the kaolin after intercalation modifying, 3h is stirred at 50 DEG C, make-methacrylic acid potassium enters interlayer, obtained monomer solution;
2) a certain amount of Potassium Persulphate and N, N is taken '-methylene-bisacrylamide, in the flask of hexanaphthene entering to be equipped with certain volume, add dispersion agent, add the monomer solution configured after abundant stirring, be warming up to 60 DEG C, copolymerzation with cross-linking reaction occurs rapidly at kaolin interlayer.
3. the preparation method of a kind of compound resin according to claim 1, is characterized in that 5) get quantitative resin, be laid in glass dish after complete swelling, slide glass be placed on gel, record slide glass upper limb height with hypsograph, take reading
l1, then 20g counterweight is placed on slide glass, the height of slide glass upper limb is recorded every 10s
l2, in triplicate, average.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410435788.9A CN105461844A (en) | 2014-08-31 | 2014-08-31 | Preparation method for composite resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410435788.9A CN105461844A (en) | 2014-08-31 | 2014-08-31 | Preparation method for composite resin |
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| Publication Number | Publication Date |
|---|---|
| CN105461844A true CN105461844A (en) | 2016-04-06 |
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| CN201410435788.9A Pending CN105461844A (en) | 2014-08-31 | 2014-08-31 | Preparation method for composite resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183566A (en) * | 2019-05-31 | 2019-08-30 | 河北民族师范学院 | A kind of compound methacrylate polymer high-intensity water absorbent agent of bentonite and preparation method thereof |
-
2014
- 2014-08-31 CN CN201410435788.9A patent/CN105461844A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183566A (en) * | 2019-05-31 | 2019-08-30 | 河北民族师范学院 | A kind of compound methacrylate polymer high-intensity water absorbent agent of bentonite and preparation method thereof |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160406 |
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| WD01 | Invention patent application deemed withdrawn after publication |