CN102516443A - Method for preparing super absorbent resin - Google Patents

Method for preparing super absorbent resin Download PDF

Info

Publication number
CN102516443A
CN102516443A CN2011104194958A CN201110419495A CN102516443A CN 102516443 A CN102516443 A CN 102516443A CN 2011104194958 A CN2011104194958 A CN 2011104194958A CN 201110419495 A CN201110419495 A CN 201110419495A CN 102516443 A CN102516443 A CN 102516443A
Authority
CN
China
Prior art keywords
parts
absorbent resin
super absorbent
water
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2011104194958A
Other languages
Chinese (zh)
Other versions
CN102516443B (en
Inventor
荣敏杰
尹献孔
许永升
付欣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Nuoer Biological Technology Co Ltd
Original Assignee
Dongying Nuoer Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dongying Nuoer Chemical Co Ltd filed Critical Dongying Nuoer Chemical Co Ltd
Priority to CN201110419495.8A priority Critical patent/CN102516443B/en
Publication of CN102516443A publication Critical patent/CN102516443A/en
Application granted granted Critical
Publication of CN102516443B publication Critical patent/CN102516443B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Polymerisation Methods In General (AREA)
  • Polymerization Catalysts (AREA)

Abstract

The invention relates to the field of polymerization water-soluble high molecular auxiliary chemicals, in particular to a method for preparing super absorbent resin. The super absorbent resin comprises the following raw materials in parts by weight: 100 to 300 parts of acrylic acid, 100 to 300 parts of caustic soda solution with the mass concentration of 25 to 50 percent, 50 to 100 parts of cross linking agent, 100 to 300 parts of deionized water, 20 to 100 parts of reinforcing agent and 0.5 to 2 parts of redox initiator. The preparation method comprises the following steps of: after adding the acrylic acid into a reactor, adding the caustic soda solution to neutralize; then adding the cross linking agent and the reinforcing agent and filling nitrogen to remove oxygen; adding the initiator to carry out polymerization at a temperature of 30 to 80 DEG C; and after the reaction is completed, obtaining colloid and pelleting, drying and crushing the colloid to obtain the super absorbent resin. The super absorbent resin prepared by the method has higher water adsorption speed and larger water adsorption times. Compared with the existing super absorbent resin, the super absorbent resin prepared by the method can have better water adsorption and water retention effects under the condition of small using amount.

Description

A kind of preparation method of High hydrophilous resin
Technical field
The present invention relates to polywater soluble macromolecular auxiliary chemicals field, relate in particular to a kind of preparation method of High hydrophilous resin.
Background technology
Water treatment field now, water quality is increasingly sophisticated, and the requirement of Water Treatment Chemicals is also improved day by day.Mostly polymer flocculant SEPIGEL 305 commonly used in the market is linear structure.It is bigger that its flocculating effect is influenced by the strong shearing action of whizzer, makes the purifying water effect variation, and adding dose increases.
Summary of the invention
The object of the invention is exactly the defective that exists to prior art, and the preparation method of the High hydrophilous resin of absorption speed that a kind of technology simply can significantly improve SAP and water retention capacity is provided.
The present invention realizes that through following technical scheme the weight part of raw material consists of: vinylformic acid 100-300, mass concentration 25-50% sodium hydroxide solution 100-300, linking agent 50-100, water 100-300, toughener 20-100, redox initiator 0.5-2; The preparation process is: after in reactor drum, adding vinylformic acid, add the sodium hydroxide solution neutralization; Add linking agent, toughener, water then, add the redox initiator initiator after the deoxygenation 30-80 ℃ of polymerization; Obtain colloid after reaction finishes and obtain High hydrophilous resin through granulation, drying, fragmentation.
Described linking agent is a N,N methylene bis acrylamide, and described toughener is a methylene-succinic acid, can significantly improve the suction multiple and the absorption speed of water-absorbing resin.
Said redox initiator is the combination of superoxide and sodium sulfite anhy 96, perhaps the combination of persulphate and sodium sulfite anhy 96.
Said superoxide is a hydrogen peroxide; Described persulphate is Potassium Persulphate or ammonium persulphate.
Described polymerization time can confirm that begin to rise to reaction starting point with temperature, temperature no longer rises to reaction end, is preferably 3-6 hour according to the real reaction situation.
The leading indicator of the High hydrophilous resin of the present invention's preparation:
Outward appearance: white particle
PH value: 6.5-7
Inhale the zero(ppm) water multiple: >=2000 times
Inhale the artificial urine multiple: >=800 times
Inhale 0.9% saline water: >=1000 times
The High hydrophilous resin of the present invention's preparation has absorption speed and bigger suction multiple faster, compares with current water-absorbing resin, can be issued to suction, water conservation effect preferably at less consumption.And have following advantage: 1) method for making is easy, and technology is simple; 2) do not use azo-initiator, no azo class material is residual, more is applicable to sanitary product; 3) introduced methylene-succinic acid, resulting resin has stronger absorption speed and stronger water retention capacity; 4), do not have " three wastes " without organic solvent.
Embodiment
Provide five exemplary embodiments below; Initiator wherein can be selected the mixture of hydrogen peroxide, ammonium persulphate and Potassium Persulphate thrin and sodium sulfite anhy 96; The concentration of sodium hydroxide solution is not limited to the concentration among the embodiment; Can suitably select, concentration is selected when higher, and the amount of deionized water can suitably reduce.
Embodiment 1
Each ingredients weight parts:
Vinylformic acid 100
50% sodium hydroxide solution 120
N,N methylene bis acrylamide 80
Deionized water 196
Methylene-succinic acid 60
Initiator 0.5
The preparation process is:
1, earlier vinylformic acid is joined in the reaction kettle;
2, neutralize with sodium hydroxide solution then;
3, add N,N methylene bis acrylamide, deionized water, methylene-succinic acid then;
4, open stirring then, and feed the high pure nitrogen deoxygenation;
5, under nitrogen protection, add initiator 50 ℃ of polymerizations 5 hours;
6, colloid obtains High hydrophilous resin through granulation, drying, fragmentation.
Embodiment 2
Each ingredients weight parts:
Vinylformic acid 90
50% sodium hydroxide solution 110
N,N methylene bis acrylamide 120
Deionized water 200
Methylene-succinic acid 100
Initiator 1.2
The preparation process is:
1, general/vinylformic acid joins in the reaction kettle earlier;
2, neutralize with sodium hydroxide solution then;
3, add N,N methylene bis acrylamide, deionized water, methylene-succinic acid then;
4, open stirring then, and feed the high pure nitrogen deoxygenation;
5, under nitrogen protection, add initiator 70 ℃ of polymerizations 4 hours;
6, colloid obtains High hydrophilous resin through granulation, drying, fragmentation.
Embodiment 3
Each ingredients weight parts:
Vinylformic acid 150
50% sodium hydroxide solution 180
N,N methylene bis acrylamide 60
Deionized water 160
Methylene-succinic acid 70
Initiator 1
The preparation process is:
1, general/vinylformic acid joins in the reaction kettle earlier;
2, neutralize with sodium hydroxide solution then;
3, add N,N methylene bis acrylamide, deionized water, methylene-succinic acid then;
4, open stirring then, and feed the high pure nitrogen deoxygenation;
5, under nitrogen protection, add initiator at 80 ℃ of polyase 13 .5 hours;
6, colloid obtains High hydrophilous resin through granulation, drying, fragmentation.
Embodiment 4
Each ingredients weight parts:
Vinylformic acid 300
50% sodium hydroxide solution 300
N,N methylene bis acrylamide 100
Deionized water 300
Methylene-succinic acid 100
Initiator 2
The preparation process is:
1, general/vinylformic acid joins in the reaction kettle earlier;
2, neutralize with sodium hydroxide solution then;
3, add N,N methylene bis acrylamide, deionized water, methylene-succinic acid then;
4, open stirring then, and feed the high pure nitrogen deoxygenation;
5, under nitrogen protection, add initiator at 80 ℃ of polyase 13s hour;
6, colloid obtains High hydrophilous resin through granulation, drying, fragmentation.
Embodiment 5
Each ingredients weight parts:
Vinylformic acid 100
50% sodium hydroxide solution 100
N,N methylene bis acrylamide 50
Deionized water 100
Methylene-succinic acid 20
Initiator 0.8
The preparation process is:
1, general/vinylformic acid joins in the reaction kettle earlier;
2, neutralize with sodium hydroxide solution then;
3, add N,N methylene bis acrylamide, deionized water, methylene-succinic acid then;
4, open stirring then, and feed the high pure nitrogen deoxygenation;
5, under nitrogen protection, add initiator 30 ℃ of polymerizations 6 hours;
6, colloid obtains High hydrophilous resin through granulation, drying, fragmentation.
Above embodiment 1-5 only is a part exemplary embodiments of the present invention, and the raw material among the present invention is carried out other combination, as long as keep proportioning raw materials and controlled variable among the present invention, the High hydrophilous resin of preparation all can reach following index:
Outward appearance: white particle
PH value: 6.5-7
Inhale the zero(ppm) water multiple: >=2000 times
Inhale the artificial urine multiple: >=800 times
Inhale 0.9% saline water: >=1000 times
Verify through actual the use; This product has been introduced new monomer, has the bigger wetting ability group of density, thereby has absorption speed faster and greater than the suction multiple of 2000ml/g; Compare with current water-absorbing resin, can be issued to suction, water conservation effect preferably at less consumption.

Claims (5)

1. the preparation method of a High hydrophilous resin is characterized in that, the weight part of raw material consists of: vinylformic acid 100-300; Mass concentration 25-50% sodium hydroxide solution 100-300, linking agent 50-100, water 100-300; Toughener 20-100, redox initiator 0.5-2; The preparation process is: after in reactor drum, adding vinylformic acid, add the sodium hydroxide solution neutralization; Add linking agent, toughener, water then, add initiator after the deoxygenation 30-80 ℃ of polymerization; The colloid that reaction obtains after finishing obtains High hydrophilous resin through granulation, drying, fragmentation.
2. the preparation method of High hydrophilous resin according to claim 1 is characterized in that, described linking agent is a N,N methylene bis acrylamide, and described toughener is a methylene-succinic acid.
3. the preparation method of High hydrophilous resin according to claim 1 is characterized in that, said redox initiator is the combination of superoxide and sodium sulfite anhy 96, perhaps the combination of persulphate and sodium sulfite anhy 96.
4. the preparation method of High hydrophilous resin according to claim 3 is characterized in that, said superoxide is a hydrogen peroxide; Described persulphate is Potassium Persulphate or ammonium persulphate.
5. according to the preparation method of the described High hydrophilous resin of the arbitrary claim of 1-4, it is characterized in that described polymerization time is 3-6 hour.
CN201110419495.8A 2011-12-15 2011-12-15 Method for preparing super absorbent resin Active CN102516443B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201110419495.8A CN102516443B (en) 2011-12-15 2011-12-15 Method for preparing super absorbent resin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201110419495.8A CN102516443B (en) 2011-12-15 2011-12-15 Method for preparing super absorbent resin

Publications (2)

Publication Number Publication Date
CN102516443A true CN102516443A (en) 2012-06-27
CN102516443B CN102516443B (en) 2014-01-01

Family

ID=46287549

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201110419495.8A Active CN102516443B (en) 2011-12-15 2011-12-15 Method for preparing super absorbent resin

Country Status (1)

Country Link
CN (1) CN102516443B (en)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102702656A (en) * 2012-07-05 2012-10-03 东营市诺尔化工有限责任公司 Preparation method of high liquid permeability water-absorbing resin
CN103214616A (en) * 2013-04-16 2013-07-24 华南理工大学 Preparation method of porous-super-absorbent resin
CN104403249A (en) * 2014-11-19 2015-03-11 山东诺尔生物科技有限公司 Preparation method of antibacterial super absorbent resin
CN104479074A (en) * 2014-11-13 2015-04-01 苏州威尔德工贸有限公司 High water-absorbing resin for diaper and preparation method thereof
CN105131208A (en) * 2015-08-13 2015-12-09 浙江省林业科学研究院 Rice husk carbon-based water retention agent preparation method and rice husk carbon-based water retention agent
CN106317280A (en) * 2016-08-22 2017-01-11 山东诺尔生物科技有限公司 Preparation method of high-expansivity water-absorbent resin for cable water-blocking tapes
CN106380536A (en) * 2016-09-19 2017-02-08 山东诺尔生物科技有限公司 Preparation method of high-polymer material for water blocking
CN109776731A (en) * 2017-11-13 2019-05-21 济南华迪工贸有限公司 A kind of preparation method of polyacrylic acid large-particle size bead-like water-absorbent resin
CN112159283A (en) * 2020-10-18 2021-01-01 山东喜美农业科技有限公司 Preparation and use methods of chitosan oligosaccharide coated slow-release fertilizer
CN112175143A (en) * 2020-10-18 2021-01-05 山东喜美农业科技有限公司 Preparation method of chitosan oligosaccharide coated sustained release agent
WO2023188633A1 (en) * 2022-03-30 2023-10-05 Sdpグローバル株式会社 Water-absorbable resin composition, absorber and absorbent article each using same, and method for producing water-absorbable resin composition

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1587289A (en) * 2004-07-09 2005-03-02 浙江大学 Process for preparing high water absorption resin
CN1624008A (en) * 2004-10-28 2005-06-08 长沙国藩科技有限公司 Colour composite high water absorbing resin and its preparation process
US20110301027A1 (en) * 2008-12-19 2011-12-08 Sca Hygiene Products Ab Superabsorbent polymer composite comprising a superabsorbent polymer and cellulosic nanofibrils

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1587289A (en) * 2004-07-09 2005-03-02 浙江大学 Process for preparing high water absorption resin
CN1624008A (en) * 2004-10-28 2005-06-08 长沙国藩科技有限公司 Colour composite high water absorbing resin and its preparation process
US20110301027A1 (en) * 2008-12-19 2011-12-08 Sca Hygiene Products Ab Superabsorbent polymer composite comprising a superabsorbent polymer and cellulosic nanofibrils

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴力立: "聚衣康酸/ 聚丙烯酸互穿网络水凝胶的研究", 《武汉理工大学学报》 *

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102702656A (en) * 2012-07-05 2012-10-03 东营市诺尔化工有限责任公司 Preparation method of high liquid permeability water-absorbing resin
CN102702656B (en) * 2012-07-05 2013-12-04 东营市诺尔化工有限责任公司 Preparation method of high liquid permeability water-absorbing resin
CN103214616A (en) * 2013-04-16 2013-07-24 华南理工大学 Preparation method of porous-super-absorbent resin
CN103214616B (en) * 2013-04-16 2015-09-02 华南理工大学 A kind of preparation method of porous-super-absorberesin resin
CN104479074A (en) * 2014-11-13 2015-04-01 苏州威尔德工贸有限公司 High water-absorbing resin for diaper and preparation method thereof
CN104403249A (en) * 2014-11-19 2015-03-11 山东诺尔生物科技有限公司 Preparation method of antibacterial super absorbent resin
CN105131208A (en) * 2015-08-13 2015-12-09 浙江省林业科学研究院 Rice husk carbon-based water retention agent preparation method and rice husk carbon-based water retention agent
CN106317280A (en) * 2016-08-22 2017-01-11 山东诺尔生物科技有限公司 Preparation method of high-expansivity water-absorbent resin for cable water-blocking tapes
CN106380536A (en) * 2016-09-19 2017-02-08 山东诺尔生物科技有限公司 Preparation method of high-polymer material for water blocking
CN109776731A (en) * 2017-11-13 2019-05-21 济南华迪工贸有限公司 A kind of preparation method of polyacrylic acid large-particle size bead-like water-absorbent resin
CN112159283A (en) * 2020-10-18 2021-01-01 山东喜美农业科技有限公司 Preparation and use methods of chitosan oligosaccharide coated slow-release fertilizer
CN112175143A (en) * 2020-10-18 2021-01-05 山东喜美农业科技有限公司 Preparation method of chitosan oligosaccharide coated sustained release agent
CN112175143B (en) * 2020-10-18 2022-03-29 山东喜美农业科技有限公司 Preparation method of chitosan oligosaccharide coated sustained release agent
CN112159283B (en) * 2020-10-18 2022-05-13 史丹利化肥(平原)有限公司 Preparation and use methods of chitosan oligosaccharide coated slow-release fertilizer
WO2023188633A1 (en) * 2022-03-30 2023-10-05 Sdpグローバル株式会社 Water-absorbable resin composition, absorber and absorbent article each using same, and method for producing water-absorbable resin composition

Also Published As

Publication number Publication date
CN102516443B (en) 2014-01-01

Similar Documents

Publication Publication Date Title
CN102516443B (en) Method for preparing super absorbent resin
CN102382264B (en) Preparation method of cellulose-based water absorbent material
CN103214616B (en) A kind of preparation method of porous-super-absorberesin resin
RU2006134597A (en) METHOD FOR PRODUCING AN ABSORBING AGENT AND AN ABSORBING AGENT
CN103044636B (en) Preparation method of enzymatically hydrolyzed sericin protein composite absorbent material
CN102702656B (en) Preparation method of high liquid permeability water-absorbing resin
CN106565913A (en) Preparation method of urea-wrapped cellulose-based super absorbent resin
CN102516455A (en) Multi-polymerization preparation method of flocculant
CN102532409A (en) Method for preparing net-shaped cationic polyacrylamide
CN104448134A (en) Method for preparing acrylamide copolymer
CN103613709A (en) Method for synthesizing special heavy metal absorption ion resin by using potato starch xanthate as raw material
CN103058561A (en) Environmentally-friendly low-energy-consumption polycarboxylic acid high-performance reducer as well as preparation method and application thereof
CN101440144A (en) Zwitterion association type high wate-absorption resin and preparing method thereof
CN105693952A (en) Natural component water-retaining agent production technology
CN104403249A (en) Preparation method of antibacterial super absorbent resin
CN102417564A (en) Water-retaining agent and preparation method thereof by papermaking sludge
CN107555567A (en) A kind of composite polyacrylamide for sewage disposal
CN104892856B (en) A kind of preparation method of polycarboxylate water-reducer
CN106279563A (en) A kind of preparation method of urine patience water-absorbing resin
CN103087252B (en) Preparation method of high-absorption composite
CN100412100C (en) Seaweed type water-absorbing-retaining material, and its preparing method
CN105384882A (en) Oxidized peat fulvic acid composite water retaining agent and preparation method thereof
CN101993516A (en) Ultraviolet light initiation preparation method of polyacrylate type composite super absorbent resin
CN103059223A (en) Method for synthesizing super absorbent resin through graft copolymerization of alpha-potato starch
CN102702405A (en) Method for preparing ultralow-residue water absorbing resins

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: SHANDONG NUOER BIOLOGICAL TECHNOLOGY CO., LTD.

Free format text: FORMER OWNER: DONGYING NUOER CHEMICAL CO., LTD.

Effective date: 20141225

C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20141225

Address after: 257333 Shandong city of Dongying province Dongying Port Economic Development Zone, east of Hong Kong Xi Liu Lu Road south of the harbour

Patentee after: SHANDONG NUOER BIOLOGICAL TECHNOLOGY Co.,Ltd.

Address before: 257333, Dongying County, Shandong province Guangrao Li magpie Industrial Park

Patentee before: Dongguan Nuoer Chemical Co.,Ltd.

PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Process for preparing high water absorption resin

Effective date of registration: 20170228

Granted publication date: 20140101

Pledgee: Weihai commercial bank Limited by Share Ltd. Dongying branch

Pledgor: SHANDONG NUOER BIOLOGICAL TECHNOLOGY Co.,Ltd.

Registration number: 2017990000133

PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20180321

Granted publication date: 20140101

Pledgee: Weihai commercial bank Limited by Share Ltd. Dongying branch

Pledgor: SHANDONG NUOER BIOLOGICAL TECHNOLOGY Co.,Ltd.

Registration number: 2017990000133

PC01 Cancellation of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Process for preparing high water absorption resin

Effective date of registration: 20180321

Granted publication date: 20140101

Pledgee: Weihai commercial bank Limited by Share Ltd. Dongying branch

Pledgor: SHANDONG NUOER BIOLOGICAL TECHNOLOGY Co.,Ltd.

Registration number: 2018990000212

PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20190125

Granted publication date: 20140101

Pledgee: Weihai commercial bank Limited by Share Ltd. Dongying branch

Pledgor: SHANDONG NUOER BIOLOGICAL TECHNOLOGY Co.,Ltd.

Registration number: 2018990000212

PC01 Cancellation of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Process for preparing high water absorption resin

Effective date of registration: 20190221

Granted publication date: 20140101

Pledgee: Weihai commercial bank Limited by Share Ltd. Dongying branch

Pledgor: SHANDONG NUOER BIOLOGICAL TECHNOLOGY Co.,Ltd.

Registration number: 2019990000081

PP01 Preservation of patent right

Effective date of registration: 20191224

Granted publication date: 20140101

PP01 Preservation of patent right
PD01 Discharge of preservation of patent
PD01 Discharge of preservation of patent

Date of cancellation: 20200824

Granted publication date: 20140101

PP01 Preservation of patent right
PP01 Preservation of patent right

Effective date of registration: 20200824

Granted publication date: 20140101

PD01 Discharge of preservation of patent
PD01 Discharge of preservation of patent

Date of cancellation: 20200824

Granted publication date: 20140101

PP01 Preservation of patent right

Effective date of registration: 20221124

Granted publication date: 20140101

PP01 Preservation of patent right