CN104072651A - Method for synthesizing polyacrylamide with high molecular weight - Google Patents
Method for synthesizing polyacrylamide with high molecular weight Download PDFInfo
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- CN104072651A CN104072651A CN201410331502.2A CN201410331502A CN104072651A CN 104072651 A CN104072651 A CN 104072651A CN 201410331502 A CN201410331502 A CN 201410331502A CN 104072651 A CN104072651 A CN 104072651A
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- polyacrylamide
- preparation
- rare earth
- earth metal
- high molecular
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Abstract
The invention discloses a method for synthesizing polyacrylamide with a high molecular weight. The method comprises the following steps: dissolving acrylamide in distilled water, stirring until acrylamide is completely dissolved, adding a compound composed of a chloride of a rare earth metal and NaHSO3 under a heating condition, stirring to react for a period of time, stopping the reaction, adding a small amount of absolute ethyl alcohol to initiate precipitation, stewing, performing vacuum filtration, washing the precipitate twice by using absolute ethyl alcohol, and drying until the mass is constant to obtain polyacrylamide with high molecular weight. Compared with the prior art, the compound composed of chloride hydrate of the rare earth metal and NaHSO3 is used as an initiator, absolute ethyl alcohol is used as a precipitation initiator, no inert atmosphere is needed, the reaction is performed in an open system under a normal temperature condition, the reaction time is short, polyacrylamide with high molecular weight has small energy source cost, the highest yield can reach 100%, and a new way is provided for batch industrial production of polyacrylamide with high molecular weight under mild conditions.
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 is because the functions such as its excellent throwing out and reduction fluid resistance 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 that polyacrylamide is synthetic, be still the little of acrylamide polymerization reaction initiator with rare earth metal.The people such as Feng Siwei, Xu Xiaodong, Chen Lingling, Zhu Yuanqi use 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 under middle high temperature, carry out, this has greatly limited production and the application of acrylamide.
Summary of the invention
For the deficiency of prior art existence, 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, by absolute ethanol washing precipitation 2 times, is dried to constant mass, obtains polyacrylamide, and wherein dehydrated alcohol consumption is 1/10th of distilled water consumption.
Described acrylamide is dissolved in distilled water, 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 that adds 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 when having a small amount of solid to separate out, stops heating, continues to be stirred to a large amount of solids and separates out, and under 50-60 DEG C of condition, is dried to constant weight, obtains SmCl
36H
2o, Sm
2o
3with the ratio of the amount of substance of hydrochloric acid be 1:6.
Described YbCl
36H
2the preparation method of O is: the La that takes 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
3with the ratio of the amount of substance of hydrochloric acid be 1:6.
Measure the relative molecular mass that the present invention prepares polyacrylamide, method is: the polymers soln with the 1.000mol NaCl 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 carried out.Then, try to achieve [η] with the software Analysis1.0 that calculates acrylamide copolymer relative molecular mass, finally by formula M=802 × [η]
1.25try to achieve the relative molecular mass of polyacrylamide.
Compare with prior art, the present invention has used chloride monohydrate and the NaHSO of rare earth metal
3the mixture of composition is initiator, and dehydrated alcohol does initiation precipitation agent, without inert atmosphere, under unlimited system, normal temperature condition, carries out, and 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%, for the acrylamide of the high molecular batch suitability for industrialized production under mild conditions provides 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 massfraction and is 16% monomer solution, be stirred to completely and dissolve, be heated to 30 DEG C, insulation, by the SmCl of preparation
36H
2o and NaHSO
3prepare pressed powder as initiator according to amount of substance than 1:4, the ratio 1:400 of initiator and the amount of substance of monomer, stir, continue reaction 1h, stopped reaction, adds 100ml dehydrated alcohol to cause precipitation, decompress filter, by absolute ethanol washing precipitation 2 times, being dried to constant mass, obtain polyacrylamide.
SmCl
36H
2the preparation method of O:
By Sm
2o
3pressed powder is dissolved in the hydrochloric acid that concentration is 6mol/L, stirs, and when being heated to a small amount of solid and separating out, stops heating, continues to be stirred to a large amount of solids and separates out, and 50 DEG C are dried to constant weight, obtain SmCl
36H
2o.
Embodiment 1-6, initiator is SmCl
36H
2o-NaHSO
3, according to carrying out under following table 1 condition.
Following table 1 has provided 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 massfraction and is 16% monomer solution, be stirred to completely and dissolve, be heated to 30 DEG C, insulation, by the YbCl of preparation
36H
2o and NaHSO
3prepare pressed powder as initiator according to amount of substance than 1:5, the ratio 1:200 of initiator and the amount of substance of monomer, stir, continue reaction 2h, stopped reaction, adds 100ml dehydrated alcohol to cause precipitation, decompress filter, by absolute ethanol washing precipitation 2 times, being dried to constant mass, obtain polyacrylamide.
Described YbCl
36H
2the preparation method of O is: the La that takes 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
3with the ratio of the amount of substance of hydrochloric acid be 1:6.
Embodiment 7-17, initiator is YbCl
36H
2o-NaHSO
3, according to carrying out under following table 2 conditions.
Following table 2 has provided 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 massfraction and is 18% monomer solution, be stirred to completely and dissolve, be heated to 30 DEG C, insulation, by the LaCl of preparation
36H
2o and NaHSO
3prepare pressed powder as initiator according to amount of substance than 1:5, the ratio 1:400 of initiator and the amount of substance of monomer, stir, continue reaction 1h, stopped reaction, adds 100ml dehydrated alcohol to cause precipitation, decompress filter, by absolute ethanol washing precipitation 2 times, being dried to constant mass, obtain polyacrylamide.
Embodiment 18-26, initiator is LaCl
36H
2o-NaHSO
3, according to carrying out under following table 3 conditions.
Following table 3 has provided 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 is the object for giving an example and illustrating just, but not is 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, all belongs in the present invention's scope required for protection.
Claims (9)
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, adds dehydrated alcohol to cause precipitation, and decompress filter after leaving standstill, by absolute ethanol washing precipitation 2 times, is dried to constant mass, obtains polyacrylamide, and wherein dehydrated alcohol consumption is 1/10th of distilled water consumption.
2. synthetic method according to claim 1, is characterized in that, described acrylamide is dissolved in distilled water, and obtaining monomer solution concentration is 14-20%.
3. preparation method according to claim 1, is characterized in that, under described heating condition, Heating temperature is 20-80 DEG C.
4. preparation 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. preparation 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. according to the preparation method described in claim 1,4 or 5 any one, it is characterized in that, the chloride monohydrate of described rare earth metal is YbCl
36H
2o, LaCl
36H
2o or SmCl
36H
2o.
7. preparation method according to claim 1, is characterized in that, after described reaction for some time, the reaction times is 0.3-10h.
8. preparation method according to claim 1, 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 when having a small amount of solid to separate out, stops heating, continues to be stirred to a large amount of solids and separates out, and under 50-60 DEG C of condition, is dried to constant weight, obtains SmCl
36H
2o, Sm
2o
3with the ratio of the amount of substance of hydrochloric acid be 1:6.
9. preparation method according to claim 2, is characterized in that, takes the La of 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
3with the ratio of the amount of substance of hydrochloric acid be 1:6.
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| CN201410331502.2A CN104072651B (en) | 2014-07-11 | 2014-07-11 | A kind of synthetic method of polyacrylamide of high molecular |
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| CN104072651B CN104072651B (en) | 2016-03-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574041A (en) * | 2018-12-28 | 2019-04-05 | 中盐淮安鸿运盐化有限公司 | A kind of lime-flue gas bittern purifying method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999051335A1 (en) * | 1998-04-06 | 1999-10-14 | Life Technologies, Inc. | Large pore volume composite mineral oxide beads, their preparation and their applications for adsorption and chromatography |
| 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 |
-
2014
- 2014-07-11 CN CN201410331502.2A patent/CN104072651B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999051335A1 (en) * | 1998-04-06 | 1999-10-14 | Life Technologies, Inc. | Large pore volume composite mineral oxide beads, their preparation and their applications for adsorption and chromatography |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574041A (en) * | 2018-12-28 | 2019-04-05 | 中盐淮安鸿运盐化有限公司 | A kind of lime-flue gas bittern purifying method |
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