CN103923289B - A kind of preparation method strengthening resin material microballoon - Google Patents
A kind of preparation method strengthening resin material microballoon Download PDFInfo
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- CN103923289B CN103923289B CN201410169653.2A CN201410169653A CN103923289B CN 103923289 B CN103923289 B CN 103923289B CN 201410169653 A CN201410169653 A CN 201410169653A CN 103923289 B CN103923289 B CN 103923289B
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- trimeric cyanamide
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Abstract
Strengthen a preparation method for resin material microballoon, it relates to a kind of preparation method strengthening resin material microballoon.The object of the invention is to solve melamine/formaldehyde resin microballoon prepared by existing method and there is adhesion problems in higher concentrations, and shape and structure is single, specific surface area is little, complete processing is complicated and the problem high to environmental requirement.Method: one, utilize furfural, deionized water and trimeric cyanamide, through being uniformly mixed and regulating pH, obtains trimeric cyanamide furfural mixed solution; Two, trimeric cyanamide furfural mixed solution is transferred to irradiation under irradiation source, obtains black trimeric cyanamide furfural reaction liquid; Three, by black trimeric cyanamide furfural through washing, ultrasonic disperse, centrifugation and drying, namely obtain trimeric cyanamide furfuryl resin ball.The present invention is mainly for the preparation of irregular spherical enhancing resin material.
Description
Technical field
The present invention relates to a kind of preparation method strengthening resin material microballoon.
Background technology
The valence link of people to various resin and the understanding of configuration have been enriched in the discovery of the resin of novel structure, excellent performance, worldwide start resin material research boom, the novel resin material of different structure and pattern is synthesized in succession, has brought the research of resin material into nanometer era.As one of focus in resin material family in recent years, resin material has the performance of the excellences such as specific tenacity is high and chemically stable is good, damping and amortization is good.Therefore be widely used in support of the catalyst, fuel cell, strongthener etc.
Trimeric cyanamide, a kind of triazines nitrogen heterocyclic ring organic compound, nitrogen content is high, special chemical structure, becomes the type material of synthesis various types of resins in recent years.The development of melamine/formaldehyde resin, melamine/formaldehyde resin ball, trimeric cyanamide/oxalic dialdehyde coating material none do not confirm this point.
Summary of the invention
The object of the invention is to solve melamine/formaldehyde microballoon prepared by existing method and there is adhesion problems in higher concentrations, and shape and structure is single, specific surface area is little, complete processing is complicated and the problem high to environmental requirement, and provide a kind of preparation method strengthening resin material microballoon.
A kind of preparation method strengthening resin material microballoon, specifically complete according to the following steps: one, first furfural is joined in deionized water, after mixing, add trimeric cyanamide, be stirred to till mixing, pH value is adjusted to 4 ~ 7 by recycling HCl, obtains trimeric cyanamide furfural mixed solution; Two, the trimeric cyanamide furfural mixed solution obtained in step one is transferred to irradiation under irradiation source, irradiation 10 ~ 30min, obtains black trimeric cyanamide furfural reaction liquid; Three, black trimeric cyanamide furfural reaction liquid step 2 obtained adopts deionized water wash 3 times, use washing with alcohol again 1 time, then ultrasonic disperse is to even, centrifugation under 5000 ~ 8000r/min condition again, it is dry 4h ~ 12h in 60 ~ 90 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains trimeric cyanamide furfuryl resin ball.
Volume ratio 1:(2 ~ 30 of the furfural described in step one and deionized water);
The volume of the furfural described in step one and the mass ratio of trimeric cyanamide are 1mL:(0.04 ~ 2) g.
Advantage of the present invention: one, the present invention have studied a kind of novel method of synthesizing enhancing resin material, and this method has opened up the visual field of synthetic resins; Two, the present invention utilizes trimeric cyanamide and the reaction of furfural under energy beam to push the development of trimeric cyanamide to a climax, improve melamine/formaldehyde microballoon prepared by existing method and there is adhesion problems in higher concentrations, and shape and structure is single, specific surface area is little, complete processing is complicated and the problem high to environmental requirement; Three, the performance of the excellence that irregular spherical carbon material specific surface area is large, porosity is high, thermally-stabilised and chemically stable is good prepared of the present invention.Compared to other synthetic methods, starting material furfural of the present invention is chosen proper, and the enhancing resin material of synthesis, increases the intensity of resin material, improves its mechanical property performance, is a kind of excellent synthetic method; Obtain in a lot of field and apply extremely widely.
Accompanying drawing explanation
Fig. 1 is scanning electronic microscope (SEM) figure of enhancing resin material prepared by test one;
Fig. 2 is the X-ray diffractogram (XRD) of enhancing resin material prepared by test one.
Embodiment
Embodiment one: present embodiment is a kind of preparation method strengthening resin material microballoon, specifically complete according to the following steps: one, first furfural is joined in deionized water, trimeric cyanamide is added after mixing, be stirred to till mixing, pH value is adjusted to 4 ~ 7 by recycling HCl, obtains trimeric cyanamide furfural mixed solution; Two, the trimeric cyanamide furfural mixed solution obtained in step one is transferred to irradiation under irradiation source, irradiation 10 ~ 30min, obtains black trimeric cyanamide furfural reaction liquid; Three, black trimeric cyanamide furfural reaction liquid step 2 obtained adopts deionized water wash 3 times, use washing with alcohol again 1 time, then ultrasonic disperse is to even, centrifugation under 5000 ~ 8000r/min condition again, it is dry 4h ~ 12h in 60 ~ 90 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains trimeric cyanamide furfuryl resin ball.
Volume ratio 1:(2 ~ 30 of the furfural described in present embodiment step one and deionized water).
The mol ratio of the trimeric cyanamide described in present embodiment step one and furfural is 1:(2 ~ 6).
Present embodiment have studied a kind of novel method of synthesizing enhancing resin material, and this method complete processing is easy, the time is short, has synthesized the enhancing resin material with high strength, thermostability and chemical stability, has opened up the visual field of synthesizing new resin.
Present embodiment utilizes trimeric cyanamide and the reaction of furfural under energy beam to push the development of trimeric cyanamide to a climax, improve melamine/formaldehyde microballoon prepared by existing method and there is adhesion problems in higher concentrations, and shape and structure is single, specific surface area is little, complete processing is complicated and the problem high to environmental requirement.
The performance of the excellence that enhancing resin material intensity is high, thermally-stabilised and chemically stable is good prepared by present embodiment.Compared to other synthetic methods, starting material furfural of the present invention is chosen proper, and the enhancing resin material of synthesis, increases the intensity of resin, is a kind of excellent synthetic method.
Embodiment two: the difference of present embodiment and embodiment one is: volume ratio 1:(10 ~ 20 of the furfural described in step one and deionized water).Other are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: the mol ratio of the trimeric cyanamide described in step one and furfural is 1:(3 ~ 5).Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the irradiation source described in step 2 is
137cs caesium source.Other are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: black trimeric cyanamide furfural reaction liquid step 2 obtained in step 3 adopts deionized water wash 3 times, use washing with alcohol again 1 time, then ultrasonic disperse is to even, centrifugation under 6000 ~ 7000r/min condition again, it is dry 4h ~ 8h in 60 ~ 80 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains trimeric cyanamide furfuryl resin ball.Other are identical with embodiment one to four.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of trimeric cyanamide furfuryl resin ball, specifically completes according to the following steps:
One, first join in 20mL deionized water by 4.5mL furfural, add 1.2g trimeric cyanamide after mixing, be stirred to till mixing, pH value is adjusted to 6 by recycling HCl, obtains trimeric cyanamide furfural mixed solution; Two, the trimeric cyanamide furfural mixed solution obtained in step one is transferred to irradiation under irradiation source, irradiation 20min, obtains black trimeric cyanamide furfural reaction liquid; Three, black trimeric cyanamide furfural reaction liquid step 2 obtained adopts deionized water wash 3 times, use washing with alcohol again 1 time, then ultrasonic disperse is to even, centrifugation under 7000r/min condition again, it is dry 12h in 80 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains trimeric cyanamide furfuryl resin ball.
Irradiation source described in this testing sequence two is
137cs caesium source.
Adopt the enhancing resin material of this test of sem observation preparation; As shown in Figure 1, Fig. 1 is scanning electronic microscope (SEM) figure of enhancing resin material prepared by test one; Characterizing resin material by Fig. 1 is microballoon, and size is homogeneous not.
X-ray diffractometer is adopted to observe the enhancing resin material of this test preparation; As shown in Figure 2, Fig. 2 is the X-ray diffractogram (XRD) of enhancing resin material prepared by test one; Have obvious diffraction peak 25.5 ° and 43.7 ° as seen in Figure 2, exosyndrome material is graphite platelet.
Test two: the application of trimeric cyanamide furfuryl resin ball, specifically carries out according to following steps: mixed with paper pulp by trimeric cyanamide furfuryl resin ball, be heating and curing.
Trimeric cyanamide furfuryl resin ball prepared by the present invention can be used as paper making intensifier and uses, due to product resin chain having a large amount of hydroxyls, after solidifying with paper pulp Hybrid Heating, can dehydration condensation be there is in resin and adjacent hydroxyl, thus reduce paper by the sliding capability soaked between rear fiber, produce certain reinforced effects.
The trimeric cyanamide furfuryl resin ball that table 1 is prepared for the present invention strengthens the contrast that the tensile strength of paper and common toughener (starch) strengthen, as can be seen from the table the advantage of trimeric cyanamide furfuryl resin ball tensile strength prepared of the present invention.
Table 1
Claims (4)
1. one kind strengthens the preparation method of resin material microballoon, it is characterized in that a kind of preparation method strengthening resin microsphere completes according to the following steps: one, first join in deionized water by furfural, trimeric cyanamide is added after mixing, be stirred to till mixing, pH value is adjusted to 4 ~ 7 by recycling HCl, obtains trimeric cyanamide furfural mixed solution; Two, the trimeric cyanamide furfural mixed solution obtained in step one is transferred to irradiation under irradiation source, irradiation 10 ~ 30min, obtains black trimeric cyanamide furfural reaction liquid; Three, black trimeric cyanamide furfural reaction liquid step 2 obtained adopts deionized water wash 2 ~ 3 times, use washing with alcohol again 1 ~ 2 time, ultrasonic disperse is to even, centrifugation under 5000 ~ 8000r/min condition again, it is dry 4h ~ 12h in 60 ~ 90 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains trimeric cyanamide furfuryl resin ball;
Volume ratio 1:(2 ~ 30 of the furfural described in step one and deionized water);
The mol ratio of the trimeric cyanamide described in step one and furfural is 1:(2 ~ 6);
Irradiation source described in step 2 is
137cs caesium source.
2. a kind of preparation method strengthening resin material microballoon according to claim 1, is characterized in that volume ratio 1:(10 ~ 20 of the furfural described in step one and deionized water).
3. a kind of preparation method strengthening resin material microballoon according to claim 1, is characterized in that the mol ratio of the trimeric cyanamide described in step one and furfural is 1:(3 ~ 5).
4. a kind of preparation method strengthening resin material microballoon according to claim 1, it is characterized in that black trimeric cyanamide furfural reaction liquid step 2 obtained in step 3 adopts deionized water wash 3 times, use washing with alcohol again 1 time, then ultrasonic disperse is to even, centrifugation under 6000 ~ 7000r/min condition again, it is dry 4h ~ 8h in 60 ~ 80 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains trimeric cyanamide furfuryl resin ball.
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| CN201410169653.2A CN103923289B (en) | 2014-04-25 | 2014-04-25 | A kind of preparation method strengthening resin material microballoon |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003074580A1 (en) * | 2002-03-02 | 2003-09-12 | Merck Patent Gmbh | Method for the production of spherical particles made of melamine resin |
| JP2004083848A (en) * | 2002-07-04 | 2004-03-18 | Nissan Chem Ind Ltd | Method for producing colored spherical composite cured melamine resin particle |
| CN102898663A (en) * | 2012-10-15 | 2013-01-30 | 杭州精彩化工有限公司 | Method for preparing thermosetting amino resin microspheres |
| CN103012706A (en) * | 2012-11-22 | 2013-04-03 | 兰州大学 | Melamine-dialdehyde condensation product and synthetic method and application thereof |
| CN103130973A (en) * | 2011-11-28 | 2013-06-05 | 同济大学 | Method for synthesizing melamine urea formaldehyde resin microsphere |
-
2014
- 2014-04-25 CN CN201410169653.2A patent/CN103923289B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003074580A1 (en) * | 2002-03-02 | 2003-09-12 | Merck Patent Gmbh | Method for the production of spherical particles made of melamine resin |
| JP2004083848A (en) * | 2002-07-04 | 2004-03-18 | Nissan Chem Ind Ltd | Method for producing colored spherical composite cured melamine resin particle |
| CN103130973A (en) * | 2011-11-28 | 2013-06-05 | 同济大学 | Method for synthesizing melamine urea formaldehyde resin microsphere |
| CN102898663A (en) * | 2012-10-15 | 2013-01-30 | 杭州精彩化工有限公司 | Method for preparing thermosetting amino resin microspheres |
| CN103012706A (en) * | 2012-11-22 | 2013-04-03 | 兰州大学 | Melamine-dialdehyde condensation product and synthetic method and application thereof |
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Inventor after: Zhang Yanhong Inventor after: Bo Zhipeng Inventor after: Bai Yingwei Inventor after: Lin Yingfang Inventor after: Sun Liguo Inventor before: Zhang Yanhong Inventor before: Bai Yingwei Inventor before: Lin Yingfang Inventor before: Sun Liguo |
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