CN104140499A - Method for preparing super absorbent polymer (SAP) from carboxymethylcellulose (CMC) and maleic acid (MA) - Google Patents

Method for preparing super absorbent polymer (SAP) from carboxymethylcellulose (CMC) and maleic acid (MA) Download PDF

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Publication number
CN104140499A
CN104140499A CN201410066212.XA CN201410066212A CN104140499A CN 104140499 A CN104140499 A CN 104140499A CN 201410066212 A CN201410066212 A CN 201410066212A CN 104140499 A CN104140499 A CN 104140499A
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China
Prior art keywords
water
absorbing resin
solution
carboxymethyl cellulose
maleic acid
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CN201410066212.XA
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Chinese (zh)
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蒋山泉
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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Priority to CN201410066212.XA priority Critical patent/CN104140499A/en
Publication of CN104140499A publication Critical patent/CN104140499A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for preparing a super absorbent polymer (SAP) from carboxymethylcellulose (CMC) and maleic acid (MA) and discloses a method for preparing the SAP. The method is characterized by comprising the steps of dissolving and mixing CMC, MA, acrylamide (AM) and a crosslinking agent, adding an initiator for polymerization and carrying out dewatering and drying, thus preparing the product, namely the super absorbent polymer. The method has the beneficial effects that the whole synthesis condition is simple; the cost is low; industrial production is safe and is easy to control; the product has stable quality and high water absorbency and is environment-friendly and pollution-free.

Description

Carboxymethyl cellulose, toxilic acid water-absorbing resin preparation method
Technical field
The present invention relates to a kind of preparation method of water-absorbing resin, especially a kind of method of preparing water-absorbing resin taking carboxymethyl cellulose (CMC), toxilic acid (MA) and acrylamide (AM) as raw material.
Background technology
Water-absorbing resin (SAP) has the high absorbent function of the heavy hundreds of of specific absorption self to several thousand times of water, and water retention property is good, becomes hydrogel once water-swelling, even if pressurization is also difficult to water to separate.Absorbent resin is that feature is the functional high molecule material with a large amount of hydrophilic radicals, is a kind of Industrial products of widespread use.Existing super absorbent resin method is mainly prepared by polymerization process by starch, carboxymethyl cellulose, vinylformic acid etc.Current water-absorbing resin raw materials is single, and price is partially expensive.Meanwhile, although existing water-absorbing resin entirety water absorbing capacity is stronger, anti-salt, temperature resistant capability is poor; Physiological saline absorbs multiple and only reaches tens times, and water sucting mechanism needs further to break through.
Summary of the invention
The concrete technical problems that the present invention will solve is how to improve toxilic acid and carboxymethyl cellulose in the application percentage of preparing in acrylic amide water-absorbing resin, and selection and the corresponding linking agent of water-absorbing resin, when its preparation cost is significantly reduced, improve further its water-intake rate, for agroforestry and industry, its objective is the preparation method that a kind of eco-friendly water-absorbing resin is provided with in a large number.
The preparation method of carboxymethyl cellulose provided by the present invention, toxilic acid and acrylamide water-absorbing resin:
(1) prepare maleic acid solution with distilled water, the swelling carboxymethyl cellulose of warm water;
(2) maleic acid solution is regulated with 25% NaOH solution, make its degree of neutralization reach 80%;
(3) carboxymethyl cellulose and acrylamide are joined in above-mentioned solution with certain mass ratio, carboxymethyl cellulose, toxilic acid and the proportion of acylamide are 1 ︰ 3 ︰ 6, by linking agent N, N '-methyl bisacrylamide joins in solution with 0.1% massfraction, reaction 10-20 minute post-heating to 45 ~ 55 DEG C, then after 5 ~ 15 minutes, obtain synthetic liquid with the speed stirring that is less than or equal to 100rpm;
(4) initiator ammonium persulfate-sodium bisulfite is joined in synthetic liquid with 0.2% massfraction, logical nitrogen protection, after reaction 4 ~ 6h, is then cooled to normal temperature, obtains hydrogel;
(5) after being dried, hydrogel obtains water-absorbing resin;
(6) water-absorbing resin is pulverized, obtained Powdered water-absorbing resin.
Brief description of the drawings
Fig. 1 is process flow sheet prepared by carboxymethyl cellulose, toxilic acid water-absorbing resin
Embodiment
By embodiment, the present invention is conducted further description and is illustrated below:
Accurately take the acrylamide of 6g and be placed in the there-necked flask of 250mL, fully stir it is uniformly dispersed; Take 3g toxilic acid, obtain solution, adding 25% NaOH solution to regulate the degree of neutralization (N) of toxilic acid is 80%; Take 1g carboxymethyl cellulose swelling with distilled water; Three kinds of monomers are mixed in the there-necked flask of 250mL, add quantitative distilled water to make w(CMC+MA+AM) quality of=20%(based on system); Add the linking agent N of massfraction 0.1%, N '-methyl bisacrylamide solution, was heated to 50 DEG C of reactions after 10 minutes, dripped massfraction 0.2% initiator ammonium persulfate-sodium sulfite solution again, continued to be stirred to mix; Pass into nitrogen and maintain 50 DEG C of reactions of constant temperature.Reaction 5h obtains water white colloid; The vacuum drying oven that colloid is placed in to 65 DEG C is dried to constant weight, and pulverizing desciccate makes the thick product of super absorbent resin; At 70 DEG C, soak thick product, stirring, washing 3 times to remove uncrosslinked homopolymer and unreacted monomer with deionized water, filter, dry, pulverize, make the absorbent resin P(CMC/MA/AM of purifying).Water absorbent rate 230g/g in pure water.

Claims (3)

1. carboxymethyl cellulose, toxilic acid water-absorbing resin preparation method, is characterized in that: prepare maleic acid solution with distilled water; Maleic acid solution is regulated with 25% NaOH, make its degree of neutralization reach 80%; By carboxymethyl cellulose, toxilic acid and acrylamide taking mass ratio as 1 ︰ 3 ︰ 6 wiring solution-formings and be placed in there-necked flask; Add again the linking agent N of 0.1% massfraction, N '-methylene-bis acryloyl solution; Be heated to 45 ~ 55 DEG C, then after 5 ~ 15 minutes, obtain synthetic liquid with the speed stirring that is less than or equal to 100rpm; Ammonium persulfate-sodium bisulfite solution is joined in synthetic liquid with 0.2% massfraction, and logical hydrogen shield, after reaction 4 ~ 6h, is then cooled to normal temperature, obtains hydrogel; After being dried, hydrogel obtains water-absorbing resin; Water-absorbing resin is pulverized, obtained Powdered water-absorbing resin.
2. preparation method as claimed in claim 1, is characterized in that, described in it, monomer mass is 1 ︰ 3 ︰ 6 than carboxymethyl cellulose, toxilic acid and acrylamide.
3. preparation method as claimed in claim 1, is characterized in that linking agent N described in it, and the add-on of N '-methylene-bisacrylamide is 0.1% of monomer mass mark.
CN201410066212.XA 2014-02-26 2014-02-26 Method for preparing super absorbent polymer (SAP) from carboxymethylcellulose (CMC) and maleic acid (MA) Pending CN104140499A (en)

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CN201410066212.XA CN104140499A (en) 2014-02-26 2014-02-26 Method for preparing super absorbent polymer (SAP) from carboxymethylcellulose (CMC) and maleic acid (MA)

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Application Number Priority Date Filing Date Title
CN201410066212.XA CN104140499A (en) 2014-02-26 2014-02-26 Method for preparing super absorbent polymer (SAP) from carboxymethylcellulose (CMC) and maleic acid (MA)

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CN104140499A true CN104140499A (en) 2014-11-12

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1290714A (en) * 2000-11-09 2001-04-11 徐月平 High hydroscopicity resin specially for oil field and agriculture
CN1651476A (en) * 2004-12-30 2005-08-10 北京科技大学 Method of oreparing starch grafting type high water absorption resin by wave polymerization
CN1766000A (en) * 2004-10-25 2006-05-03 罗学刚 Environment friendly lignin resin of high water absorbence and its preparation method
CN101200519A (en) * 2007-11-23 2008-06-18 武汉理工大学 Modification method of acroleic acid macromolecular absorbent resin salt tolerance
CN101787101A (en) * 2010-01-25 2010-07-28 陕西科技大学 Preparation method of nanometer resin with high hygroscopy
CN101864036A (en) * 2010-06-03 2010-10-20 济南大学 Method for synthesizing super absorbent resin by plant straw
CN102633944A (en) * 2012-03-31 2012-08-15 陕西科技大学 Preparation method of salt-tolerance controlled-release high-water-absorption resin with hydrophobic chain segments

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1290714A (en) * 2000-11-09 2001-04-11 徐月平 High hydroscopicity resin specially for oil field and agriculture
CN1766000A (en) * 2004-10-25 2006-05-03 罗学刚 Environment friendly lignin resin of high water absorbence and its preparation method
CN1651476A (en) * 2004-12-30 2005-08-10 北京科技大学 Method of oreparing starch grafting type high water absorption resin by wave polymerization
CN101200519A (en) * 2007-11-23 2008-06-18 武汉理工大学 Modification method of acroleic acid macromolecular absorbent resin salt tolerance
CN101787101A (en) * 2010-01-25 2010-07-28 陕西科技大学 Preparation method of nanometer resin with high hygroscopy
CN101864036A (en) * 2010-06-03 2010-10-20 济南大学 Method for synthesizing super absorbent resin by plant straw
CN102633944A (en) * 2012-03-31 2012-08-15 陕西科技大学 Preparation method of salt-tolerance controlled-release high-water-absorption resin with hydrophobic chain segments

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
SHANQUAN JIANG, ET AL.: "Preparation and properties of Anti-salt Super Absorbent Resin", 《ADVANCED MATERIALS RESEARCH》 *
于智 等: "羧甲基纤维素钠接枝共聚制备高吸水性树脂", 《沈阳化工大学学报》 *
张春涛 等: "羧甲基纤维素钠接枝AA/AM/SSS高吸水树脂的制备", 《化工新型材料》 *
申艳敏 等: "CMC和AA/AM三元共聚高吸水树脂的研究", 《辽宁化工》 *
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