CN105542071A - Method for preparing composite nanometer hydrogel precursor - Google Patents
Method for preparing composite nanometer hydrogel precursor Download PDFInfo
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- CN105542071A CN105542071A CN201610053845.6A CN201610053845A CN105542071A CN 105542071 A CN105542071 A CN 105542071A CN 201610053845 A CN201610053845 A CN 201610053845A CN 105542071 A CN105542071 A CN 105542071A
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- Prior art keywords
- precursor
- hydrogel
- carbon source
- carbon
- hydrogel precursor
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 23
- 239000002243 precursor Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 229930006000 Sucrose Natural products 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 11
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 4
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 238000004448 titration Methods 0.000 claims abstract description 4
- 239000005720 sucrose Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 235000013681 dietary sucrose Nutrition 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
- 229960004793 sucrose Drugs 0.000 abstract 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Colloid Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention provides a method for preparing a composite nanometer hydrogel precursor. An acrylamide lattice reagent and an ammonium persulfate initiator are stirred for 30 min, a set quantity of a saccharose carbon source is added, the molar ratio of carbon to aluminum atoms is 6, and a precursor mixing solution is obtained after stirring is performed at low temperature for 1 h. An ammonia solution with the concentration ratio being 1:2 is titrated into the mixing solution at the dripping speed of 3-5 ml/min, and continuous stirring is performed for 2 h after titration is finished. After stirring is performed, polymerization is performed at the temperature of 65 DEG C to obtain the composite nanometer hydrogel precursor. The obtained hydrogel is directly placed into a drying oven to be dried, and the precursor is obtained after drying is performed. Saccharose is adopted as a carbon source for preparing the hydrogel precursor, it is ensured that the precursor can be evenly dispersed, the defect that layering is caused when activated carbon is used as a carbon source is overcome, the obtained precursor is good in using performance, and the method is suitable for preparing the hydrogel precursor.
Description
Technical field
What the present invention proposed is chemical field process control method, specifically prepares the method for composite Nano hydrogel precursor.
Background technology
In chemical industry, widely use hydrogel at present, and use hydrogel to participate in chemical reaction as presoma, usually in hydrogel, add gac carbon source, and the presoma made exists demixing phenomenon, affect result of use.
Summary of the invention
In order to overcome existing hydrogel precursor demixing phenomenon, the present invention proposes the method preparing composite Nano hydrogel precursor.The method using sucrose as carbon source, prepares presoma by composite aquogel.Solve the technical problem that composite aquogel presoma carbon source selects to ensure presoma uniformity coefficient.
The scheme that technical solution problem of the present invention adopts is:
Acrylamide lattice reagent and ammonium persulfate initiator, after stirring 30min, add the sucrose carbon source of set amount, and carbon and aluminium atomic molar, than being C/Al=6, after low temperature 1h, obtain presoma mixed solution.Be ammonia soln the dripping in this mixed solution of speed instillation with 3 ~ 5ml/min of 1:2 by concentration ratio, titration terminates rear continuation and stirs 2h.Stir rear 65 DEG C of polymerizations and obtain composite Nano hydrogel.The hydrogel of gained is directly put into baking oven dry, after oven dry, obtain presoma.
Positively effect, the present invention adopts sucrose to be carbon source, prepares hydrogel precursor, can ensure that presoma is dispersed, and overcome the defect using gac as carbon source layering, prepared presoma use properties is excellent.The suitable method application as preparing hydrogel precursor.
Accompanying drawing explanation
Fig. 1 is present invention process procedure chart.
Embodiment
According to the figure, in the aluminum nitrate solution of the 0.3mol/l of frozen water temperature control, add acrylamide monomer, methylene radical acrylamide lattice reagent and ammonium persulfate initiator, after stirring 30min, add the sucrose carbon source of set amount, carbon is C/Al=6 with aluminium atomic molar ratio, after low temperature 1h, obtain presoma mixed solution, be ammonia soln the dripping in this mixed solution of speed instillation with 3 ~ 5ml/min of 1:2 by concentration ratio, titration terminates rear continuation and stirs 2h, stirs rear 65 DEG C of polymerizations and obtains composite Nano hydrogel.The hydrogel of gained is directly put into baking oven dry, after oven dry, obtain presoma.
Feature:
In presoma, take ammoniacal liquor as the condition of precipitation agent, setting network proportioning, carbon al mole ratio is 6, is that carbon source synthesizes presoma respectively with sucrose.Take sucrose as carbon source, aluminium and carbon mix.
Sucrose carbon atom can be evenly distributed in the three-dimensional net structure that aluminum oxide formed.Contained element is Al element, O element, C element, N element, and carbon and aluminium atom are evenly distributed.
Experiment proves:
Adopt sucrose or gac to be carbon source in experiment respectively, adopt polymer-network gel process synthesis presoma.It is carbon source that research finds with sucrose, and aluminium source and carbon mix; And be carbon source with gac, there is obvious demixing phenomenon in AlN presoma.The control of this composite Nano hydrogel techniques solves the mixing non-uniform phenomenon that traditional method prepares synthetics.
Claims (1)
1. prepare the method for composite Nano hydrogel precursor, it is characterized in that: in the aluminum nitrate solution of the 0.3mol/l of frozen water temperature control, add acrylamide monomer, methylene radical acrylamide lattice reagent and ammonium persulfate initiator, after stirring 30min, add the sucrose carbon source of set amount, carbon and aluminium atomic molar are than being C/Al=6, after low temperature 1h, obtain presoma mixed solution, be ammonia soln the dripping in this mixed solution of speed instillation with 3 ~ 5ml/min of 1:2 by concentration ratio, titration terminates rear continuation and stirs 2h, stirs rear 65 DEG C of polymerizations and obtains composite Nano hydrogel; The hydrogel of gained is directly put into baking oven dry, after oven dry, obtain presoma.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610053845.6A CN105542071A (en) | 2016-01-27 | 2016-01-27 | Method for preparing composite nanometer hydrogel precursor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610053845.6A CN105542071A (en) | 2016-01-27 | 2016-01-27 | Method for preparing composite nanometer hydrogel precursor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105542071A true CN105542071A (en) | 2016-05-04 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610053845.6A Pending CN105542071A (en) | 2016-01-27 | 2016-01-27 | Method for preparing composite nanometer hydrogel precursor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105542071A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116876109A (en) * | 2023-08-21 | 2023-10-13 | 哈尔滨工业大学 | Graphene composite fiber and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429031A (en) * | 2008-12-11 | 2009-05-13 | 沈阳大学 | Macromolecule network preparation method for high-purity ultra-fine aluminum nitride ceramic |
| CN104402452A (en) * | 2014-10-31 | 2015-03-11 | 中国航空工业集团公司基础技术研究院 | Aluminum nitride ceramic powder preparation method |
| CN104741046A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Method for preparing aluminum oxide/carbon aerogel composite material |
-
2016
- 2016-01-27 CN CN201610053845.6A patent/CN105542071A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429031A (en) * | 2008-12-11 | 2009-05-13 | 沈阳大学 | Macromolecule network preparation method for high-purity ultra-fine aluminum nitride ceramic |
| CN104741046A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Method for preparing aluminum oxide/carbon aerogel composite material |
| CN104402452A (en) * | 2014-10-31 | 2015-03-11 | 中国航空工业集团公司基础技术研究院 | Aluminum nitride ceramic powder preparation method |
Non-Patent Citations (1)
| Title |
|---|
| R.NARASIMMAN，等: "Preparation of low density carbon foams by foaming molten sucrose using an aluminium nitrate blowing agent", 《CARBON》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116876109A (en) * | 2023-08-21 | 2023-10-13 | 哈尔滨工业大学 | Graphene composite fiber and preparation method thereof |
| CN116876109B (en) * | 2023-08-21 | 2024-04-12 | 哈尔滨工业大学 | Graphene composite fiber and preparation method thereof |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Liuyan Inventor after: Zhang Ning Inventor before: Wang Liuyan |
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| COR | Change of bibliographic data | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160628 Address after: 110000 Liaoning Province, Shenyang City District wanghuanan Street No. 21 Shenyang University Shenyang City Applicant after: Shenyang Univ. Address before: 110000 Liaoning Province, Shenyang City District wanghuanan Street No. 21, Shenyang University Applicant before: Wang Liuyan |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160504 |
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| RJ01 | Rejection of invention patent application after publication |