CN102351997A - Preparation of lignin polyacrylonitrile water absorbent - Google Patents
Preparation of lignin polyacrylonitrile water absorbent Download PDFInfo
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- CN102351997A CN102351997A CN 201110195410 CN201110195410A CN102351997A CN 102351997 A CN102351997 A CN 102351997A CN 201110195410 CN201110195410 CN 201110195410 CN 201110195410 A CN201110195410 A CN 201110195410A CN 102351997 A CN102351997 A CN 102351997A
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- xylogen
- polyacrylonitrile
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- lignin
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Abstract
The invention discloses a preparation process of a lignin polyacrylonitrile water absorbent. The water absorbent takes lignin as a raw material which is capable of raising the water retention capability of lignin in a soil improvement system and endowing the biodegradable property of the lignin polyacrylonitrile water absorbent. The water absorbency of a lignin polyacrylonitrile graft copolymer is about 1-50 times. The preparation of the invention has the advantages that the preparation method is simple, the prepared water absorbent has good graininess, the slow-released moisture can be maintained for 24 hours after rapidly absorbing water, thereby the moisture retention of the agricultural sterile soil and the requirement for soil improvement can be satisfied. The water absorbent has no sorption effect to urea after water adsorption is saturated, and ensures that the fertilizer used for agriculture is completely absorbed by plants.
Description
Technical field
The invention belongs to filed of functional, particularly a kind of can the suction preserved moisture and the technology of preparing of the biodegradable xylogen polyacrylonitrile water-retaining agent of good air permeability.
Background technology
Exhausted day by day along with fossil energy, and the understanding of problems such as human environmental pollution and crisis of resource deepens continuously, the renewable character that natural polymer had comes into one's own day by day.The resource utilization of waste and the utilization of renewable resources are the key subjects of contemporary economy and society development.Xylogen is the natural high moleculer eompound that enriches, and also is the main sub product of pulp and paper industry simultaneously.Pulp and paper industry will be isolated about 1.4 hundred million tons of Mierocrystalline celluloses every year from plant, obtain the xylogen sub product about 3,000 ten thousand tons simultaneously.The xylogen cost is lower; Xylogen and verivate thereof have multiple functional; Can be used as dispersion agent, sorbent material/strippant, petroleum recovery auxiliary agent, asphalt emulsifier; Xylogen is to the human kind sustainable development major contribution organic substance source that just is to provide stable, continues the most, and its application prospect is very wide.
Up to the present, the application of art quality mostly is used with the form of sulfonated lignin.In spissated papermaking wastewater, add formaldehyde and process the xylogen formaldehyde resin; Add sulphur, zinc oxide, Triple Pressed Stearic Acid, vulcanizing agent, vulcanization accelerator, vulcanization activator and rubber more in proportion and vulcanize at a certain temperature, can make in the rubber and to fill a large amount of xylogen and still need not add tenderizer.Both solve the papermaking wastewater problem of environmental pollution, and made full use of the biomass resource waste and save a large amount of rubber again, had society and economic benefit.Xylogen is a kind of irregular net(high)polymer of three-dimensional space of phenol type phenyl-propane structural unit, have with soil in the similar performance of soil ulmin.
Summary of the invention
The invention provides a kind of technology of preparing of xylogen polyacrylonitrile water-retaining agent, improve the water retention capacity of xylogen in the soil improvement system, give xylogen polyacrylonitrile water-retaining agent biodegradable character.Preparation technology is simple for this method, and is cheap.
The preparation method of xylogen polyacrylonitrile provided by the invention, its preparation process feature is: the solvent of xylogen behind the purifying and 10-50 times of weight was stirred 1-3 hour at 50-90 ℃, and reaction is cooled to room temperature after finishing; Acrylonitrile monemer room temperature reaction 1-5 hour that adds xylogen initiator and 5-15 times weight again; Dropwise add the homopolymerization initiator again; The suspension reaction system is incubated at a certain temperature, after reaction finishes, leaves standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers.
Above-mentioned xylogen is alkali lignin, sulfonated lignin.
Above-mentioned xylogen initiator is one or more systems of ferrous sulfate and ammonium persulphate, ferrous sulfate and hydrogen peroxide, ammonium cerous sulfate and ethanol or Red copper oxide and hydrogen peroxide.
Above-mentioned homopolymerization initiator is one or more of ammonium cerous sulfate, ceric ammonium nitrate, ammonium persulphate, Potassium Persulphate or potassium permanganate.
The invention has the advantages that the preparation method is simple, the water-retaining agent graininess of preparation is good, after quick suction, keeps 24h slowly-releasing moisture, can satisfy preserving moisture and the needs of soil improvement of agriculture lean soil.This water-retaining agent to the adsorption that urea has no, can guarantee that agricultural fertilizer is all absorbed by plant after suction is saturated.
Description of drawings
The Fourier's infrared spectrum and the X-ray diffraction spectrogram of xylogen polyacrylonitrile have been provided in the Figure of description.
Fourier's infrared spectrum of Fig. 1 xylogen, xylogen polyacrylonitrile.
The X-ray diffraction spectrogram of Fig. 2 xylogen, xylogen polyacrylonitrile.
Embodiment
Instance 1
The purifying of raw material: with the NaOH solution dissolving of raw material, remove ash content and impurity in the raw material, regulate the pH value at the HCl that uses 2mol/L and be 2, filter with 2mol/L; Be washed with distilled water to neutrality; Do not see that with silver nitrate solution check white opacity is advisable, 40 ℃ of vacuum-dryings, subsequent use.
Xylogen 1.5g behind the purifying is added in the 150mL there-necked flask, add 50g zero(ppm) water and stirred 2 hours at 90 ℃, reaction is cooled to room temperature after finishing; Added ferrous sulfate 0.1g and hydrogen peroxidase 10 .3g and 0.5g acrylonitrile monemer room temperature reaction again 1 hour; Dropwise add 1.94 ceric ammonium nitrate solutions again, the suspension reaction system is at 30 ℃ of condition insulation 1h, after reaction finishes; Leave standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers, and its water absorbent rate is 4.23 times of xylogen.
The infrared spectrum of xylogen and xylogen polyacrylonitrile graft copolymers is seen accompanying drawing 1.By knowing 2930cm among the figure
-1And 2860cm
-1It is the stretching vibration peak of methyl and methylene radical; Xylogen 1720cm before the reaction
-1Absorption peak disappear, think aldehyde radical or ester bond in the lignin structure, behind graft reaction, disappear.The xylogen polyacrylonitrile is at 1600cm
-1, 1500cm
-1And 1450cm
-1The phenyl ring characteristic absorbance more obvious than xylogen.1663cm
-1Ownership is the stretching vibration of the two keys of C=N of xylogen vinyl cyanide.1600,1545,1465cm
-1The place is the skeletal vibration that belongs to phenyl ring.Xylogen is at 3436cm
-1It is the free hydroxyl group peak; The xylogen polyacrylonitrile reduces in this peak position absorption intensity, and peak value appears at 3334cm
-1, think that xylogen generation graft copolymerization causes, has confirmed Fe among the 2.4.1
2+/ H
2O
2System is correct as causing on the phenolic hydroxyl group that catalyst reaction course graft reaction occurs in xylogen.Fig. 3-3 can know 10-50 ° of scope, only near 20 °, have broad peak and peak height value to be more or less the same; The peak position of xylogen polyacrylonitrile is 21.7 °; 19.64 ° of the peak positions of xylogen show that the crystal content of xylogen polyacrylonitrile and crystal grain are all little, explain that also the xylogen polyacrylonitrile is improving the absorptive while; Still kept the unordered characteristic of lignin molecule, so the space between this material granule is still bigger.
Xylogen 2.5g behind the purifying is added in the 150mL there-necked flask, add 50g zero(ppm) water and stirred 2 hours at 90 ℃, reaction is cooled to room temperature after finishing; Added ferrous sulfate 0.1g and hydrogen peroxidase 10 .3g and 0.5g acrylonitrile monemer room temperature reaction again 1 hour; Dropwise add 1.94 ceric ammonium nitrate solutions again, the suspension reaction system is at 30 ℃ of condition insulation 1h, after reaction finishes; Leave standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers, and its water absorbent rate is 3.02 times of xylogen.
Xylogen 2.5g behind the purifying is added in the 150mL there-necked flask, add 50g zero(ppm) water and stirred 2 hours at 90 ℃, reaction is cooled to room temperature after finishing; Added ferrous sulfate 0.1g and hydrogen peroxidase 10 .3g and 0.5g acrylonitrile monemer room temperature reaction again 1 hour; Dropwise add 1.94 ceric ammonium nitrate solutions again, the suspension reaction system is at 30 ℃ of condition insulation 2h, after reaction finishes; Leave standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers, and its water absorbent rate is 3.1 times of xylogen.
Instance 4
Xylogen 2.5g behind the purifying is added in the 150mL there-necked flask, add 50g zero(ppm) water and stirred 2 hours at 90 ℃, reaction is cooled to room temperature after finishing; Added ferrous sulfate 0.1g and hydrogen peroxidase 10 .3g and 0.5g acrylonitrile monemer room temperature reaction again 1 hour; Dropwise add 1.94 ceric ammonium nitrate solutions again, the suspension reaction system is at 30 ℃ of condition insulation 3h, after reaction finishes; Leave standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers, and its water absorbent rate is 1.88 times of xylogen.
Instance 5
Xylogen 2.5g behind the purifying is added in the 150mL there-necked flask, add 50g zero(ppm) water and stirred 2 hours at 90 ℃, reaction is cooled to room temperature after finishing; Added ferrous sulfate 0.1g and hydrogen peroxidase 10 .3g and 0.5g acrylonitrile monemer room temperature reaction again 1 hour; Dropwise add 1.94 ceric ammonium nitrate solutions again, the suspension reaction system is at 40 ℃ of condition insulation 2h, after reaction finishes; Leave standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers, and its water absorbent rate is 2.45 times of xylogen.
Instance 6
Xylogen 2.0g behind the purifying is added in the 150mL there-necked flask, add 50g zero(ppm) water and stirred 2 hours at 90 ℃, reaction is cooled to room temperature after finishing; Added ferrous sulfate 0.1g and hydrogen peroxidase 10 .3g and 0.5g acrylonitrile monemer room temperature reaction again 1 hour; Dropwise add 1.94 ceric ammonium nitrate solutions again, the suspension reaction system is at 30 ℃ of condition insulation 1h, after reaction finishes; Leave standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers, and its water absorbent rate is 2.47 times of xylogen.
Claims (4)
1. the technology of preparing of xylogen polyacrylonitrile water-retaining agent, the preparation process is following:
The solvent of xylogen behind the purifying and 10-50 times of weight was stirred 1-3 hour at 50-90 ℃, and reaction is cooled to room temperature after finishing; Acrylonitrile monemer room temperature reaction 1-5 hour that adds xylogen initiator and 5-15 times weight again; Dropwise add the homopolymerization initiator again; The suspension reaction system is incubated at a certain temperature, after reaction finishes, leaves standstill, filtration, hot wash solid product; Remove the homopolymer in the graftomer with the washing of N-N N again, centrifugal, drying makes the xylogen polyacrylonitrile graft copolymers.
2. xylogen polyacrylonitrile water-retaining agent according to claim 1 is characterized in that: xylogen is alkali lignin, sulfonated lignin.
3. xylogen polyacrylonitrile water-retaining agent according to claim 1 is characterized in that: the xylogen initiator is ferrous sulfate and ammonium persulphate, ferrous sulfate and hydrogen peroxide, ammonium cerous sulfate and ethanol or Red copper oxide and hydrogen peroxide.
4. xylogen polyacrylonitrile water-retaining agent according to claim 1 is characterized in that: the homopolymerization initiator is ammonium cerous sulfate, ceric ammonium nitrate, ammonium persulphate, Potassium Persulphate or potassium permanganate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110195410 CN102351997A (en) | 2011-07-13 | 2011-07-13 | Preparation of lignin polyacrylonitrile water absorbent |
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| CN 201110195410 CN102351997A (en) | 2011-07-13 | 2011-07-13 | Preparation of lignin polyacrylonitrile water absorbent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558440A (en) * | 2013-10-24 | 2015-04-29 | 中国科学院兰州化学物理研究所 | Preparation method of lignin grafted copolymer |
| CN106577708A (en) * | 2016-11-29 | 2017-04-26 | 广西南岜仔科技有限公司 | Novel herbicide |
| CN110061239A (en) * | 2018-03-20 | 2019-07-26 | 南方科技大学 | Lignin-base binder and preparation method thereof and lithium ion battery |
| CN112537989A (en) * | 2020-11-10 | 2021-03-23 | 衡水市中禾谷盐碱地生态研究所 | Preparation method of lignin biomass resin-based saline-alkali soil improver |
-
2011
- 2011-07-13 CN CN 201110195410 patent/CN102351997A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《华东石油学院学报》 19880331 王鹤义等 木质素-丙烯腈接枝共聚物及其水解产物 第132-136页 1-4 第12卷, 第1期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558440A (en) * | 2013-10-24 | 2015-04-29 | 中国科学院兰州化学物理研究所 | Preparation method of lignin grafted copolymer |
| CN104558440B (en) * | 2013-10-24 | 2017-04-05 | 中国科学院兰州化学物理研究所 | A kind of preparation method of lignin-graft copolymer |
| CN106577708A (en) * | 2016-11-29 | 2017-04-26 | 广西南岜仔科技有限公司 | Novel herbicide |
| CN110061239A (en) * | 2018-03-20 | 2019-07-26 | 南方科技大学 | Lignin-base binder and preparation method thereof and lithium ion battery |
| CN112537989A (en) * | 2020-11-10 | 2021-03-23 | 衡水市中禾谷盐碱地生态研究所 | Preparation method of lignin biomass resin-based saline-alkali soil improver |
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Application publication date: 20120215 |