CN105037726A - Synthetic method for environment-friendly polyaspartate super absorbent resin - Google Patents
Synthetic method for environment-friendly polyaspartate super absorbent resin Download PDFInfo
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- CN105037726A CN105037726A CN201510439398.3A CN201510439398A CN105037726A CN 105037726 A CN105037726 A CN 105037726A CN 201510439398 A CN201510439398 A CN 201510439398A CN 105037726 A CN105037726 A CN 105037726A
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- super absorbent
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- absorbent resin
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- polysuccinimide
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Abstract
The invention relates to the field of resin synthesis, and discloses a synthetic method for environment-friendly polyaspartate super absorbent resin. According to the synthetic method, polysuccinimide and dimethylformamide are used as raw materials, hexamethylenediamine is used as a cross-linking agent, and phosphoric acid or polyphosphoric acid is used as a catalyst. By means of the synthetic method for the environment-friendly polyaspartate super absorbent resin, the problems that existing super absorbent materials are not prone to degradation, large in residual monomer, low in water absorption and the like are solved.
Description
Technical field
The present invention relates to resins synthesis field, particularly relate to a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin.
Background technology
Poly aspartic acid (PASP) is in recent years at the green chemical that global sales increases day by day, and it is a kind of polyamino acid with carboxylic acid side chain, and fully biodegradable is environmentally friendly.In industrial today, environmental problem more and more causes the attention of people, and the Synthesis and application of poly aspartic acid enjoys the concern of countries in the world.
Poly aspartic acid Application Areas is very extensive, and it can change the crystalline structure of calcium salt, is a kind of excellent dirt dispersion agent, for recirculating cooling water system, boiler and oil-field water process; Poly aspartic acid has good viscosity reduction effect; Poly aspartic acid, can Promoting plant growth as fertilizer synergist; Poly aspartic acid also has excellent performance of keeping humidity, for the manufacture of daily cosmetics and health-care product; Super absorbent resin can be prepared by poly aspartic acid; Prepared by poly aspartic acid has been widely used on birth control, the medicine such as antitumor to solid support material; Can prepare super absorbent resin by poly aspartic acid, resin with superhigh hydroscopicity can absorb water tens times and even thousands of times at short notice, can widespread use and health product, agriculture and garden, desert prevent and treat and multiple field such as afforestation.
In sum, a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin is provided, solves the problems such as current high absorbency material is not easily degraded, monomer residue is large, water-intake rate is low, seem especially important.
Summary of the invention
The object of the invention is the deficiency existed for prior art, provide a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin, solve the problems such as current high absorbency material is not easily degraded, monomer residue is large, water-intake rate is low.
In order to solve the problems of the technologies described above, the invention provides a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin, comprising the following steps:
S1, be raw material with aspartic acid, add catalyst mix, at 150-300 DEG C, react 0.5-15h, thermal condensation forms polysuccinimide;
S2, be dissolved in dimethyl formamide by the polysuccinimide in step S1, controlling bath temperature is 60 DEG C, stirring and dissolving; Add diamine crosslinker under room temperature, at 35 DEG C, react 12h, form crosslinked polysuccinimide;
S3, the product in described step S2 is carried out suction filtration, washing, and be dispersed in 80g water, with basic solution hydrolysis, regulate pH to neutral; Then add ethanol deswelling, obtain product in 80 DEG C of dry 10h.
Wherein, the catalyzer in described step S1 is phosphoric acid, polyphosphoric acid or sulfuric acid, and described catalyst charge and aspartic acid mass ratio are 0.01-1:1.
Particularly, the quality of the polysuccinimide in described step S2 and the mass ratio of dimethyl formamide are 1:4.
Further, the molecular weight of the polysuccinimide in described step S2 is 36000 ~ 112000.
Further, the diamine crosslinker in described step S2 is diamines or quadrol.
Preferably, the concentration of described diamine crosslinker is 1.5 ~ 3%.
Preferably, the basic solution in described step S3 is aqueous sodium hydroxide solution.
Application the present invention, has following beneficial effect:
(1) the present invention adopts aspartic acid to be raw material, and the product of preparation is easily degraded, little to environmental hazard.
(2) aspartic acid super absorbent resin of the present invention has higher water-intake rate, and when polysuccinimide molecular weight is 67500 and hexanediamine concentration is 1.5%, water-intake rate is up to 1480g/g.
(3) present invention process is simple, lower to equipment requirements, with low cost.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite of not making creative work, all belongs to the scope of protection of the invention.
Embodiment 1
Present embodiment discloses a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin, take aspartic acid as raw material, add the mixing of phosphoric acid, polyphosphoric acid or sulfuric acid catalyst, described catalyst charge and aspartic acid mass ratio are 0.01-1:1, at 150-300 DEG C, react 0.5-15h, thermal condensation forms polysuccinimide; The polysuccinimide being 76500 by described 10g molecular weight is dissolved in 40g dimethyl formamide, and controlling bath temperature is 60 DEG C, stirring and dissolving; Add the hexanediamine linking agent that concentration is 1.5% under room temperature, at 35 DEG C, react 12h, form crosslinked polysuccinimide; Product is carried out suction filtration, washing, and is dispersed in 80g water, with sodium hydroxide solution hydrolysis, regulate pH to neutral; Then add ethanol deswelling, obtain product in 80 DEG C of dry 10h.
Embodiment 2
Present embodiment discloses a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin, take aspartic acid as raw material, add the mixing of phosphoric acid, polyphosphoric acid or sulfuric acid catalyst, described catalyst charge and aspartic acid mass ratio are 0.01-1:1, at 150-300 DEG C, react 0.5-15h, thermal condensation forms polysuccinimide; The polysuccinimide being 76500 by described 10g molecular weight is dissolved in 40g dimethyl formamide, and controlling bath temperature is 60 DEG C, stirring and dissolving; Add the ethylene diamine linker that concentration is 2.0% under room temperature, at 35 DEG C, react 12h, form crosslinked polysuccinimide; Product is carried out suction filtration, washing, and is dispersed in 80g water, with sodium hydroxide solution hydrolysis, regulate pH to neutral; Then add ethanol deswelling, obtain product in 80 DEG C of dry 10h.
Embodiment 3
Present embodiment discloses a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin, take aspartic acid as raw material, add the mixing of phosphoric acid, polyphosphoric acid or sulfuric acid catalyst, described catalyst charge and aspartic acid mass ratio are 0.01-1:1, at 150-300 DEG C, react 0.5-15h, thermal condensation forms polysuccinimide; The polysuccinimide being 112000 by described 10g molecular weight is dissolved in 40g dimethyl formamide, and controlling bath temperature is 60 DEG C, stirring and dissolving; Add the diamine crosslinker that concentration is 1.5% under room temperature, at 35 DEG C, react 12h, form crosslinked polysuccinimide; Product is carried out suction filtration, washing, and is dispersed in 80g water, with sodium hydroxide solution hydrolysis, regulate pH to neutral; Then add ethanol deswelling, obtain product in 80 DEG C of dry 10h.
Embodiment 4
Present embodiment discloses a kind of synthetic method of environmentally friendly poly-asparagus fern super absorbent resin, take aspartic acid as raw material, add the mixing of phosphoric acid, polyphosphoric acid or sulfuric acid catalyst, described catalyst charge and aspartic acid mass ratio are 0.01-1:1, at 150-300 DEG C, react 0.5-15h, thermal condensation forms polysuccinimide; The polysuccinimide being 112000 by described 10g molecular weight is dissolved in 40g dimethyl formamide, and controlling bath temperature is 60 DEG C, stirring and dissolving; Add the ethylene diamine linker that concentration is 2.0% under room temperature, at 35 DEG C, react 12h, form crosslinked polysuccinimide; Product is carried out suction filtration, washing, and is dispersed in 80g water, with sodium hydroxide solution hydrolysis, regulate pH to neutral; Then add ethanol deswelling, obtain product in 80 DEG C of dry 10h.
By the determination test analysis of imbibition multiple, embodiment 1 is optimum embodiment of the present invention, and resin water absorbent rate is 1480g/g.
Application the present invention, has following beneficial effect:
(1) the present invention adopts aspartic acid to be raw material, and the product of preparation is easily degraded, little to environmental hazard.
(2) aspartic acid super absorbent resin of the present invention has higher water-intake rate, and when polysuccinimide molecular weight is 67500 and hexanediamine concentration is 1.5%, water-intake rate is up to 1480g/g.
(3) present invention process is simple, lower to equipment requirements, with low cost.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (7)
1. a synthetic method for environmentally friendly poly-asparagus fern super absorbent resin, is characterized in that, comprise the following steps:
S1, be raw material with aspartic acid, add catalyst mix, at 150-300 DEG C, react 0.5-15h, thermal condensation forms polysuccinimide;
S2, be dissolved in dimethyl formamide by the polysuccinimide in step S1, controlling bath temperature is 60 DEG C, stirring and dissolving; Add diamine crosslinker under room temperature, at 35 DEG C, react 12h, form crosslinked polysuccinimide;
S3, the product in described step S2 is carried out suction filtration, washing, and be dispersed in 80g water, with basic solution hydrolysis, regulate pH to neutral; Then add ethanol deswelling, obtain product in 80 DEG C of dry 10h.
2. the synthetic method of environmentally friendly poly-asparagus fern super absorbent resin according to claim 1, it is characterized in that, the catalyzer in described step S1 is phosphoric acid, polyphosphoric acid or sulfuric acid, and described catalyst charge and aspartic acid mass ratio are 0.01-1:1.
3. the synthetic method of environmentally friendly poly-asparagus fern super absorbent resin according to claim 1 and 2, it is characterized in that, the quality of the polysuccinimide in described step S2 and the mass ratio of dimethyl formamide are 1:4.
4. the synthetic method of environmentally friendly poly-asparagus fern super absorbent resin according to claim 3, is characterized in that, the molecular weight of the polysuccinimide in described step S2 is 36000 ~ 112000.
5. the synthetic method of the environmentally friendly poly-asparagus fern super absorbent resin according to claim 1,2 or 4, is characterized in that, the diamine crosslinker in described step S2 is diamines or quadrol.
6. the synthetic method of environmentally friendly poly-asparagus fern super absorbent resin according to claim 5, is characterized in that, the concentration of described diamine crosslinker is 1.5 ~ 3%.
7. the synthetic method of environmentally friendly poly-asparagus fern super absorbent resin according to claim 6, it is characterized in that, the basic solution in described step S3 is aqueous sodium hydroxide solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510439398.3A CN105037726A (en) | 2015-07-23 | 2015-07-23 | Synthetic method for environment-friendly polyaspartate super absorbent resin |
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| CN201510439398.3A CN105037726A (en) | 2015-07-23 | 2015-07-23 | Synthetic method for environment-friendly polyaspartate super absorbent resin |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113246A (en) * | 1994-05-16 | 1995-12-13 | 三菱化学株式会社 | Acidic amino acid resin |
| US5998492A (en) * | 1994-09-13 | 1999-12-07 | Donlar Corporation | Super-absorbing polymeric networks |
| JP2000063511A (en) * | 1997-02-07 | 2000-02-29 | Mitsui Chemicals Inc | Production of crosslinked polyamino acid |
| JP2000290381A (en) * | 1999-04-08 | 2000-10-17 | Dainippon Ink & Chem Inc | Production of water-absorbent resin |
-
2015
- 2015-07-23 CN CN201510439398.3A patent/CN105037726A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113246A (en) * | 1994-05-16 | 1995-12-13 | 三菱化学株式会社 | Acidic amino acid resin |
| US5998492A (en) * | 1994-09-13 | 1999-12-07 | Donlar Corporation | Super-absorbing polymeric networks |
| JP2000063511A (en) * | 1997-02-07 | 2000-02-29 | Mitsui Chemicals Inc | Production of crosslinked polyamino acid |
| JP2000290381A (en) * | 1999-04-08 | 2000-10-17 | Dainippon Ink & Chem Inc | Production of water-absorbent resin |
Non-Patent Citations (2)
| Title |
|---|
| 冷一欣 等: "环境友好型聚天冬高吸水性树脂的合成", 《精细与专用化学品》 * |
| 杨德红 等: "《绿色化学》", 31 January 2008, 黄河水利出版社 * |
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Application publication date: 20151111 |