CN104072651B - A kind of synthetic method of polyacrylamide of high molecular - Google Patents
A kind of synthetic method of polyacrylamide of high molecular Download PDFInfo
- Publication number
- CN104072651B CN104072651B CN201410331502.2A CN201410331502A CN104072651B CN 104072651 B CN104072651 B CN 104072651B CN 201410331502 A CN201410331502 A CN 201410331502A CN 104072651 B CN104072651 B CN 104072651B
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- China
- Prior art keywords
- synthetic method
- polyacrylamide
- rare earth
- earth metal
- nahso
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Links
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 23
- 238000010189 synthetic method Methods 0.000 title claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 239000003999 initiator Substances 0.000 abstract description 15
- 230000000977 initiatory effect Effects 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229920006322 acrylamide copolymer Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of synthetic method of polyacrylamide of high molecular, comprise the following steps: acrylamide is dissolved in distilled water, is stirred to and dissolves completely, under heating condition, add muriate and the NaHSO of rare earth metal
3the mixture of composition, after stirring reaction for some time, stopped reaction, add a small amount of dehydrated alcohol and cause precipitation, decompress filter after leaving standstill, precipitate 2 times with absolute ethanol washing, be dried to constant mass, secure satisfactory grades sub-weight polyacrylamide.Compare with prior art, present invention uses chloride monohydrate and the NaHSO of rare earth metal
3the mixture of composition is initiator, dehydrated alcohol does initiation precipitation agent, without the need to inert atmosphere, carry out under unlimited system, normal temperature condition, reaction times is short, gained polyacrylamide high molecular, few energy expenditure, productive rate can reach 100%, and the acrylamide bulk industrial in a mild condition for high molecular is produced and provided new way.
Description
Technical field
The present invention relates to organic synthesis field, be specifically related to a kind of synthetic method of polyacrylamide of high molecular.
Background technology
Polyacrylamide due to its excellence throwing out and reduce the function such as fluid resistance and obtain a wide range of applications in the fields such as paper industry, petroleum industry, mining industry, metallurgical industry, medicine industry.The synthetic method of polyacrylamide has aqueous solution polymerization, letex polymerization, radio polymerization, instaneous polymerization gasification desolventizing method etc.
In prior art, a lot of to the research of polyacrylamide synthesis, but be the little of acrylamide polymerization reaction initiator with rare earth metal.The people such as Feng Siwei, Xu Xiaodong, Chen Lingling, Zhu Yuanqi with trifluoromethyl sulfonic acid as catalyst acrylamide polymerization.But above-mentioned initiator system all needs nitrogen protection in the process of initiation reaction, generally also must carry out under middle high temperature, this greatly limits production and the application of acrylamide.
Summary of the invention
For the deficiency that prior art exists, the invention provides a kind of synthetic method of polyacrylamide of high molecular, utilize a kind of chloride monohydrate and NaHSO of novel acrylamide initiator system-rare earth metal
3the mixture of composition is initiator.
The synthetic method of the polyacrylamide of a kind of high molecular provided by the invention, specifically comprises the following steps:
Acrylamide is dissolved in distilled water, after dissolving completely, under heating condition, adds chloride monohydrate and the NaHSO of rare earth metal
3the mixture of composition, stirs, and after reaction for some time, adds dehydrated alcohol, and decompress filter after leaving standstill, precipitate 2 times with absolute ethanol washing, be dried to constant mass, obtain polyacrylamide, wherein dehydrated alcohol consumption is 1/10th of distilled water consumption.
Describedly be dissolved in distilled water by acrylamide, obtaining monomer solution mass concentration is 14-20%;
Under described heating condition, Heating temperature is 20-80 DEG C;
Described chloride monohydrate and the NaHSO adding rare earth metal
3the mixture of composition, the chloride monohydrate of rare earth metal and NaHSO
3the ratio of amount of substance be 1:2-6;
The chloride monohydrate of rare earth metal and NaHSO
3the ratio of the mixture of composition and the amount of substance of acrylamide is 1:200-400;
The chloride monohydrate of described rare earth metal is YbCl
36H
2o, LaCl
36H
2o or SmCl
36H
2o.
After described reaction for some time, the reaction times is 0.3-10h.
Wherein, SmCl
36H
2the preparation method of O is: by Sm
2o
3pressed powder is dissolved in 6mol/L hydrochloric acid, stirs, and heating evaporation, to when having a small amount of solid to separate out, stops heating, continues to be stirred to a large amount of solid and separates out, be dried to constant weight, obtain SmCl under 50-60 DEG C of condition
36H
2o, Sm
2o
3be 1:6 with the ratio of the amount of substance of hydrochloric acid.
Described YbCl
36H
2the preparation method of O is: the La taking certain mass
2o
3, with slow evaporation crystallization after dissolving with hydrochloric acid, under 50-60 DEG C of condition, be dried to constant weight, airtight preservation, for subsequent use, La
2o
3be 1:6 with the ratio of the amount of substance of hydrochloric acid.
Measure the relative molecular mass that the present invention prepares polyacrylamide, method is: with the polymers soln of the 1.000molNaCl aqueous solution as solvent preparation 0.05%, the elution time of the determination of ubbelohde viscometer NaCl aqueous solution and polymers soln at 30 DEG C.Concrete operations are pressed GB12005.1-89 and are performed.Then, try to achieve [η], finally by formula M=802 × [η] with the software Analysis1.0 calculating acrylamide copolymer relative molecular mass
1.25try to achieve the relative molecular mass of polyacrylamide.
Compare with prior art, present invention uses chloride monohydrate and the NaHSO of rare earth metal
3the mixture of composition is initiator, and dehydrated alcohol does initiation precipitation agent, and without the need to inert atmosphere, carry out under unlimited system, normal temperature condition, the reaction times is short, gained polyacrylamide high molecular.Reaction conditions gentleness of the present invention, high-level efficiency, few equipment investment, few energy expenditure, unit time output is large, and productive rate can reach 100%, and the acrylamide bulk industrial in a mild condition for high molecular is produced and provided new way.
Embodiment
Embodiment 1
A synthetic method for the polyacrylamide of high molecular, comprises the following steps:
191g acrylamide is dissolved in 1000ml distilled water, is prepared into the monomer solution that massfraction is 16%, is stirred to and dissolves completely, be heated to 30 DEG C, insulation, by the SmCl of preparation
36H
2o and NaHSO
3pressed powder is prepared as initiator than 1:4 according to amount of substance, the ratio 1:400 of initiator and the amount of substance of monomer, stir, continue reaction 1h, stopped reaction, add 100ml dehydrated alcohol and cause precipitation, decompress filter, precipitate 2 times with absolute ethanol washing, be dried to constant mass, obtaining polyacrylamide.
SmCl
36H
2the preparation method of O:
By Sm
2o
3it is in the hydrochloric acid of 6mol/L that pressed powder is dissolved in concentration, stirs, and when being heated to the precipitation of a small amount of solid, stops heating, and continue to be stirred to a large amount of solid and separate out, 50 DEG C are dried to constant weight, obtain SmCl
36H
2o.
Embodiment 1-6, initiator is SmCl
36H
2o-NaHSO
3, carry out according under following table 1 condition.
Following table 1 gives reaction conditions and the result of embodiment 1-6
Table 1
Embodiment 7
A synthetic method for the polyacrylamide of high molecular, comprises the following steps:
191g acrylamide is dissolved in 1000ml distilled water, is prepared into the monomer solution that massfraction is 16%, is stirred to and dissolves completely, be heated to 30 DEG C, insulation, by the YbCl of preparation
36H
2o and NaHSO
3pressed powder is prepared as initiator than 1:5 according to amount of substance, the ratio 1:200 of initiator and the amount of substance of monomer, stir, continue reaction 2h, stopped reaction, add 100ml dehydrated alcohol and cause precipitation, decompress filter, precipitate 2 times with absolute ethanol washing, be dried to constant mass, obtaining polyacrylamide.
Described YbCl
36H
2the preparation method of O is: the La taking certain mass
2o
3, with slow evaporation crystallization after dissolving with hydrochloric acid, under 60 DEG C of conditions, be dried to constant weight, airtight preservation, for subsequent use, La
2o
3be 1:6 with the ratio of the amount of substance of hydrochloric acid.
Embodiment 7-17, initiator is YbCl
36H
2o-NaHSO
3, carry out according under following table 2 condition.
Following table 2 gives reaction conditions and the result of embodiment 7-17.
Table 2
Embodiment 18
A synthetic method for the polyacrylamide of high molecular, comprises the following steps:
215g acrylamide is dissolved in 1000ml distilled water, is prepared into the monomer solution that massfraction is 18%, is stirred to and dissolves completely, be heated to 30 DEG C, insulation, by the LaCl of preparation
36H
2o and NaHSO
3pressed powder is prepared as initiator than 1:5 according to amount of substance, the ratio 1:400 of initiator and the amount of substance of monomer, stir, continue reaction 1h, stopped reaction, add 100ml dehydrated alcohol and cause precipitation, decompress filter, precipitate 2 times with absolute ethanol washing, be dried to constant mass, obtaining polyacrylamide.
Embodiment 18-26, initiator is LaCl
36H
2o-NaHSO
3, carry out according under following table 3 condition.
Following table 3 gives reaction conditions and the result of embodiment 18-26.
Table 3
The present invention is illustrated by above-mentioned case study on implementation, but should be understood that, above-mentioned case study on implementation just for the object of illustrating and illustrate, and is not intended to the present invention to be limited within the scope of described case study on implementation.The present invention is not limited to above-mentioned case study on implementation, can also make the modification of many kinds according to instruction of the present invention, within all belonging to the present invention's scope required for protection.
Claims (8)
1. a synthetic method for the polyacrylamide of high molecular, is characterized in that, described synthetic method comprises the following steps:
Acrylamide is dissolved in distilled water, after dissolving completely, under heating condition, adds chloride monohydrate and the NaHSO of rare earth metal
3the mixture of composition, stirs, and after reaction for some time, add dehydrated alcohol and cause precipitation, decompress filter after leaving standstill, precipitate 2 times with absolute ethanol washing, be dried to constant mass, obtain polyacrylamide, wherein dehydrated alcohol consumption is 1/10th of distilled water consumption.
2. synthetic method according to claim 1, is characterized in that, described by acrylamide
Be dissolved in distilled water, obtaining monomer solution concentration is 14-20%.
3. synthetic method according to claim 1, is characterized in that, under described heating condition, Heating temperature is 20-80 DEG C.
4. synthetic method according to claim 1, is characterized in that, under described heating condition, described in add chloride monohydrate and the NaHSO of rare earth metal
3the mixture of composition, the chloride monohydrate of rare earth metal and NaHSO
3the ratio of amount of substance be 1:2-6.
5. synthetic method according to claim 4, is characterized in that, the chloride monohydrate of rare earth metal and NaHSO
3the mixture of composition is 1:200-400 with the ratio of the amount of substance of acrylamide.
6. the synthetic method according to claim 1,4 or 5 any one, is characterized in that, the chloride monohydrate of described rare earth metal is YbCl
36H
2o, LaCl
36H
2o or SmCl
36H
2o.
7. synthetic method according to claim 1, is characterized in that, after described reaction for some time, the reaction times is 0.3-10h.
8. synthetic method according to claim 6, is characterized in that, SmCl
36H
2the preparation method of O is: by Sm
2o
3pressed powder is dissolved in 6mol/L hydrochloric acid, stirs, and heating evaporation, to when having a small amount of solid to separate out, stops heating, continues to be stirred to a large amount of solid and separates out, be dried to constant weight, obtain SmCl under 50-60 DEG C of condition
36H
2o, Sm
2o
3be 1:6 with the ratio of the amount of substance of hydrochloric acid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935272A (en) * | 2010-08-18 | 2011-01-05 | 中国海洋石油总公司 | Rare earth type water-base gel crosslinking agent and preparation method thereof |
| CN103242594A (en) * | 2013-05-14 | 2013-08-14 | 中国科学院长春应用化学研究所 | Polymer hydrogel microspheres and preparation method thereof |
| CN103289102A (en) * | 2013-06-08 | 2013-09-11 | 长春理工大学 | Dual-response magnetic nano particle with fluorescence and preparation method thereof |
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| US6613234B2 (en) * | 1998-04-06 | 2003-09-02 | Ciphergen Biosystems, Inc. | Large pore volume composite mineral oxide beads, their preparation and their applications for adsorption and chromatography |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935272A (en) * | 2010-08-18 | 2011-01-05 | 中国海洋石油总公司 | Rare earth type water-base gel crosslinking agent and preparation method thereof |
| CN103242594A (en) * | 2013-05-14 | 2013-08-14 | 中国科学院长春应用化学研究所 | Polymer hydrogel microspheres and preparation method thereof |
| CN103289102A (en) * | 2013-06-08 | 2013-09-11 | 长春理工大学 | Dual-response magnetic nano particle with fluorescence and preparation method thereof |
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