CN102649833B - Method for preparing superabsorbent resin based on waste woody plant branches - Google Patents
Method for preparing superabsorbent resin based on waste woody plant branches Download PDFInfo
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- CN102649833B CN102649833B CN201210143427.8A CN201210143427A CN102649833B CN 102649833 B CN102649833 B CN 102649833B CN 201210143427 A CN201210143427 A CN 201210143427A CN 102649833 B CN102649833 B CN 102649833B
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- 239000011347 resin Substances 0.000 title claims abstract description 45
- 229920005989 resin Polymers 0.000 title claims abstract description 45
- 239000002699 waste material Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000007605 air drying Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 241000196324 Embryophyta Species 0.000 claims description 21
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 14
- 239000002023 wood Substances 0.000 claims description 14
- 240000000249 Morus alba Species 0.000 claims description 10
- 235000008708 Morus alba Nutrition 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000004160 Ammonium persulphate Substances 0.000 claims description 5
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 5
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 5
- 238000010559 graft polymerization reaction Methods 0.000 claims description 5
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical compound OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- 244000166124 Eucalyptus globulus Species 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000010413 gardening Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 125000002015 acyclic group Chemical group 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000002745 absorbent Effects 0.000 description 10
- 239000002250 absorbent Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 241000255789 Bombyx mori Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 229920000247 superabsorbent polymer Polymers 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for preparing superabsorbent resin based on waste woody plant branches. The method comprises the following steps: washing the waste woody plant branches completely, drying, crushing by using a plant crushing machine, filtering by using a screen to obtain branch powder, placing the branch powder into deionized water, heating and maintaining the temperature, introducing nitrogen all the time and stirring; after adding an initiator, adding acyclic acid neutralized by ammonium hydrogen carbonate and acrylamide sequentially, adding a crosslinking agent, adjusting the deionized water content of the whole reaction, and conducting reaction to obtain brown yellow gel; and taking out the brown yellow gel, cutting into blocks, washing with water, and performing forced air drying at a certain temperature to obtain the superabsorbent resin. The waste woody plant branches are not subjected to further chemical treatment; the process is simple and environment-friendly; the raw materials have wide sources; high-value reutilization of the agricultural and forestry waste resources is realized; and the method has the characteristics of low cost, biodegradability and high water absorbency and is applicable in the fields of agriculture, gardening, hygiene care and the like.
Description
Technical field
The present invention relates to a kind of method of preparing High hydrophilous resin, particularly relate to a kind of method of preparing High hydrophilous resin based on waste wood plants shoots.
Background technology
High hydrophilous resin is a kind of new functional macromolecule material with tridimensional network, can absorb deadweight hundred times and arrive the moisture of thousands of times, has the title of " super strength water absorbent "; Therefore appropriately crosslinked tridimensional network makes again its moisture absorbing can not adopt general physical method to extrude, and has good water retention capacity, is widely used in agricultural, gardening, hygiene care, medicine and the field such as industrial.
The demand of current whole world super absorbent resin increases progressively with annual 8%～10% speed, and wherein polyacrylic High hydrophilous resin output accounts for 80% of whole world High hydrophilous resin production, becomes the main product of this industry.But the monomer of polyacrylic is mainly derived from day by day exhausted petroleum resources, and synthetic polymkeric substance is difficult to be decomposed by the microorganism in soil, therefore a large amount of uses easily cause the very big pollution to environment after discarding.Chinese patent (CN 101864036A) " utilizes the method for straw synthesizing super absorbent resin " just take the stalk of plant and prepares High hydrophilous resin as raw material; Chinese patent (CN 101864036A) " eco-friendly lignin High hydrophilous resin and preparation method thereof " is introduced high purity lignin in super absorbent resin resin system; Chinese patent (CN101638456) " a kind of take yam starch there is the method for the High hydrophilous resin of crosslinking structure as raw material preparation " and United States Patent (USP) (US007423106B2) " Superabsorbent polymer product and use in agriculture ") all take starch and obtain High hydrophilous resin as raw material graft copolymerization propenyl monomer.At present, yet there are no and use waste wood plants shoots as macromolecular skeleton raw material, prepare maturation process or the correlation technique of High hydrophilous resin.
China Shi Ge agricultural big country, the annual agriculture and forestry organic waste material producing approximately has 6.5 hundred million to 700,000,000 tons.Wherein most of discarded farm-forestry crop directly burns or throws aside in physical environment for a long time, if do not add rational utilization and processing, not only causes the significant wastage of resource, and has a strong impact on atmospheric environment.In 400,000 tons/year of mulberry branch Wei Li， China cocoon yields, need about 8,000,000 mu of mulberry fields that mulberry leaf are provided, can produce more than 177 ten thousand tons of discarded branches per year.The main purpose that mulberry tree is cultivated is at present to feed silkworm for obtaining mulberry leaf, and few to the exploitation of ramulus mori, mainly as dried firewood burning or direct heap, abandons.In Woody plant branch, contain the macromolecular polysaccharides such as Mierocrystalline cellulose, hemicellulose and lignin; there is potential using value; therefore the high-valued recycling approach of, finding waste wood plants shoots is of great immediate significance to protection of the environment, the high-valued recycling that realizes resource.
Summary of the invention
In order to overcome, existing High hydrophilous resin biodegradability is poor, production cost is higher, water absorbent rate is lower and the low inferior problem of existing waste wood plants shoots utilization ratio, the object of this invention is to provide a kind of method of preparing High hydrophilous resin based on waste wood plants shoots.
For achieving the above object, technical scheme of the present invention is to adopt following steps:
1) waste wood plants shoots is cleaned, is dried, then pulverize with plant pulverizer, through 100 eye mesh screens, filter, obtain the branch powder that particle diameter is less than or equal to 0.15mm;
2) the branch powder obtaining in step 1) is placed in to deionized water, the mass ratio of branch powder and deionized water is 1:20 ~ 30;
3) mixture of branch powder and deionized water is heated, stir 5 ~ 30 minutes, Heating temperature is 50 ~ 70 ℃, and passes into nitrogen;
4) keep 50 ~ 70 ℃ of Heating temperatures and pass under nitrogen, add initiator after 5 ~ 20 minutes, add successively again vinylformic acid and acrylamide through bicarbonate of ammonia neutralization to carry out graft polymerization, add again linking agent and adjust the deionized water content of whole reaction and after the mass ratio of branch powder is 30 ~ 40:1, then react and within 2-3 hour, obtain brown color gel;
5) the brown color gel described in taking-up step 4), and stripping and slicing, washing, then forced air drying at 60 ~ 100 ℃, obtain High hydrophilous resin.
Described initiator is ammonium persulphate, and the mass ratio of initiator and branch powder is 0.05～0.2:1; Bicarbonate of ammonia and acrylic acid mole ratio are 0.6～0.9:1; Without the vinylformic acid of percarbonic acid hydrogen ammonium neutralization and the mass ratio of acrylamide, be 1:1～4:1; The vinylformic acid neutralizing without percarbonic acid hydrogen ammonium and the summation of acrylamide and the mass ratio of branch powder are 4～10:1; Linking agent is N,N methylene bis acrylamide, and the mass ratio of linking agent and branch powder is 0.02～0.05:1.
Described waste wood plants shoots is mulberry branch, poplar-branch or eucalyptus branch.
Compare with background technology, the beneficial effect that the present invention has is:
(1) the present invention adopts waste wood plants shoots, through cleaning, after dry, directly pulverizes as synthesizing super absorbent resin main raw material, does not need further chemical treatment, technique simply, environmental protection and starting material wide material sources;
(2) the present invention introduces waste wood plants shoots in High hydrophilous resin, realized the high-valued recycling of farm-forestry crop waste resource, what preparation cost was lower, biodegradable, water absorbing properties is comparatively excellent, be applicable to the High hydrophilous resin in the fields such as agricultural, gardening and hygiene care.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 2 High hydrophilous resin B.
Fig. 2 is the water absorbent rate of embodiment 2 High hydrophilous resin B in deionized water curve over time.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
embodiment 1:
1) discarded mulberry branch is cleaned, is dried, then pulverize with plant pulverizer, through 100 eye mesh screens, filter, obtain the mulberry branch powder that particle diameter is less than or equal to 0.15mm;
2) the mulberry branch powder 1g obtaining in step 1) is placed in to 25ml deionized water;
3) mixture of branch powder and deionized water is heated, stir 15 minutes, Heating temperature is 70 ℃, and passes into nitrogen;
4) keep 70 ℃ of Heating temperatures and pass under nitrogen, in the mixture of branch powder and deionized water, add after 10 min of ammonium persulphate 0.15g, in 3.2g vinylformic acid, add 2.2g bicarbonate of ammonia to neutralize, to add and carry out graft polymerization through the vinylformic acid that obtains of neutralization and 0.8g acrylamide successively, add again N, N-methylene-bisacrylamide 0.03g and adjust deionized water content to 40 ml of whole reaction after react again 2 hours, obtain brown color gel;
5) the brown color gel described in taking-up step 4), and stripping and slicing, washing, then forced air drying at 60 ℃, obtain High hydrophilous resin A.
embodiment 2:
1) discarded poplar-branch is cleaned, is dried, then pulverize with plant pulverizer, through 100 eye mesh screens, filter, obtain the branch powder that particle diameter is less than or equal to 0.15mm;
2) the 1g branch powder obtaining in step 1) is placed in to 20ml deionized water;
3) mixture of branch powder and deionized water is heated, stir 30 minutes, Heating temperature is 60 ℃, and passes into nitrogen;
4) keep 60 ℃ of Heating temperatures and pass under nitrogen, in the mixture of branch powder and deionized water, add after 20 min of ammonium persulphate 0.2g, in 4g vinylformic acid, add 3.3g bicarbonate of ammonia to neutralize, to add and carry out graft polymerization through the vinylformic acid that obtains of neutralization and 2g acrylamide successively, add again N, N-methylene-bisacrylamide 0.05g and adjust deionized water content to 30 ml of whole reaction after react again 2.5 hours, obtain brown color gel;
5) the brown color gel described in taking-up step 4), and stripping and slicing, washing, then forced air drying at 100 ℃, obtain High hydrophilous resin B.
embodiment 3:
1) discarded eucalyptus branch is cleaned, is dried, then pulverize with plant pulverizer, through 100 eye mesh screens, filter, obtain the branch powder that particle diameter is less than or equal to 0.15mm;
2) the branch powder 1g obtaining in step 1) is placed in to 30ml deionized water;
3) mixture of branch powder and deionized water is heated, stir 5 minutes, Heating temperature is 50 ℃, and passes into nitrogen;
4) keep 50 ℃ of Heating temperatures and pass under nitrogen, in the mixture of branch powder and deionized water, add after 5 min of ammonium persulphate 0.05g, in 5g vinylformic acid, add 4.8g bicarbonate of ammonia to neutralize, to add and carry out graft polymerization through the vinylformic acid that obtains of neutralization and 5g acrylamide successively, add again N, N-methylene-bisacrylamide and adjust deionized water content to 35 ml of whole reaction after react again 3 hours, obtain brown color gel;
5) the brown color gel described in taking-up step 4), and stripping and slicing, washing, then forced air drying at 80 ℃, obtain High hydrophilous resin C.
The water absorbing properties of three kinds of High hydrophilous resins that mensuration embodiment 1,2,3 prepares in deionized water, tap water and 0.9%NaCl salt solution.Table 1 is the water absorbent rate test result after being absorbed water 2 hours by the prepared High hydrophilous resin of embodiment 1,2,3.As known from Table 1, adopt High hydrophilous resin A, the B of preparation method's gained of the present invention, the water absorbent rate of C all has good water absorbing properties, wherein the water absorbent rate of High hydrophilous resin B is the most excellent, its multiplying power that absorbs deionized water, tap water, salt solution reaches respectively 575 g/g, 288 g/g and 70 g/g, meets the feature of High hydrophilous resin.
As Fig. 1, from the scanning electron microscope (SEM) photograph of High hydrophilous resin B, can find out, the surface arrangement of this High hydrophilous resin cavity and pit.These cavities and pit can improve the area of High hydrophilous resin and contact with moisture, are conducive to absorb fast moisture, thereby improve the rate of water absorption of High hydrophilous resin.
As Fig. 2, the High hydrophilous resin B that can find out this different-grain diameter obtaining after crushed has different rate of water absorption, it is saturated that 16-20 object High hydrophilous resin can reach water suction in 20min, and that more than less 80 orders of particle diameter High hydrophilous resin just can reach water suction in only in 2min is saturated, this illustrates that this High hydrophilous resin has rate of water absorption faster.
Table 1
What more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (2)
1. based on waste wood plants shoots, prepare a method for High hydrophilous resin, it is characterized in that comprising the following steps:
1) waste wood plants shoots is cleaned, is dried, then pulverize with plant pulverizer, through 100 eye mesh screens, filter, obtain the branch powder that particle diameter is less than or equal to 0.15mm;
2) the branch powder obtaining in step 1) is placed in to deionized water, the mass ratio of branch powder and deionized water is 1:20 ~ 30;
3) mixture of branch powder and deionized water is heated, stir 5 ~ 30 minutes, Heating temperature is 50 ~ 70 ℃, and passes into nitrogen;
4) keep 50 ~ 70 ℃ of Heating temperatures and pass under nitrogen, add initiator after 5 ~ 20 minutes, add successively again vinylformic acid and acrylamide through bicarbonate of ammonia neutralization to carry out graft polymerization, add again linking agent and adjust the deionized water content of whole reaction and after the mass ratio of branch powder is 30 ~ 40:1, then react and within 2-3 hour, obtain brown color gel;
5) the brown color gel described in taking-up step 4), and stripping and slicing, washing, then forced air drying at 60 ~ 100 ℃, obtain High hydrophilous resin;
Described initiator is ammonium persulphate, and the mass ratio of initiator and branch powder is 0.05～0.2:1; Bicarbonate of ammonia and acrylic acid mole ratio are 0.6～0.9:1; Without the vinylformic acid of percarbonic acid hydrogen ammonium neutralization and the mass ratio of acrylamide, be 1:1～4:1; The vinylformic acid neutralizing without percarbonic acid hydrogen ammonium and the summation of acrylamide and the mass ratio of branch powder are 4～10:1; Linking agent is N,N methylene bis acrylamide, and the mass ratio of linking agent and branch powder is 0.02～0.05:1.
2. a kind of method of preparing High hydrophilous resin based on waste wood plants shoots according to claim 1, is characterized in that: described waste wood plants shoots is mulberry branch, poplar-branch or eucalyptus branch.
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| CN106589243A (en) * | 2016-11-09 | 2017-04-26 | 浙江理工大学 | Preparation method of bio-base superabsorbent resin composite absorbent core material |
| CN106905489A (en) * | 2017-02-10 | 2017-06-30 | 同济大学 | The method that a kind of utilization food market waste dish prepares water-loss reducer of soil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058626A (en) * | 2007-05-11 | 2007-10-24 | 陕西科技大学 | Method of preparing high water absorption resin |
| CN101864036A (en) * | 2010-06-03 | 2010-10-20 | 济南大学 | Method for synthesizing super absorbent resin by plant straw |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058626A (en) * | 2007-05-11 | 2007-10-24 | 陕西科技大学 | Method of preparing high water absorption resin |
| CN101864036A (en) * | 2010-06-03 | 2010-10-20 | 济南大学 | Method for synthesizing super absorbent resin by plant straw |
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