CN109369833A - A method of Sodium Polyacrylate is prepared by ternary initiator system - Google Patents
A method of Sodium Polyacrylate is prepared by ternary initiator system Download PDFInfo
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- CN109369833A CN109369833A CN201811261868.1A CN201811261868A CN109369833A CN 109369833 A CN109369833 A CN 109369833A CN 201811261868 A CN201811261868 A CN 201811261868A CN 109369833 A CN109369833 A CN 109369833A
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- Prior art keywords
- parts
- initiator
- sodium polyacrylate
- weight
- neutralizer
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- 239000003999 initiator Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 title claims abstract description 20
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 title claims abstract description 20
- 239000011734 sodium Substances 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 17
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- USYAMXSCYLGBPT-UHFFFAOYSA-L 3-carboxy-3-hydroxypentanedioate;tin(2+) Chemical compound [Sn+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O USYAMXSCYLGBPT-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- LXEKPEMOWBOYRF-UHFFFAOYSA-N [2-[(1-azaniumyl-1-imino-2-methylpropan-2-yl)diazenyl]-2-methylpropanimidoyl]azanium;dichloride Chemical compound Cl.Cl.NC(=N)C(C)(C)N=NC(C)(C)C(N)=N LXEKPEMOWBOYRF-UHFFFAOYSA-N 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 abstract description 16
- 229920000642 polymer Polymers 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 229910002567 K2S2O8 Inorganic materials 0.000 description 3
- 229910004882 Na2S2O8 Inorganic materials 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229940047670 sodium acrylate Drugs 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002562 thickening agent Substances 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
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
Abstract
The present invention relates to the field of polymers, especially a kind of method that Sodium Polyacrylate is prepared by ternary initiator system.The present invention is added dropwise 140-185 parts of lye when cooling down, obtains neutralizer the following steps are included: (1) by weight, 100 parts of acrylic acid are added in 80-100 part of distilled water；(2) then by weight filtering neutralizer sequentially adds 5-12.5 parts of medium temperature initiator, 1 part of high-temperature initiator, 1% 1-3 parts of stannous citrate acid sodium, 4.5-7.5 parts of low temperature initiators in filtrate, stirs evenly, obtain mixed liquor；(3) mixed liquor reacts 4h at 25-30 DEG C, then dries, and obtains product.Step of the invention is simple and convenient to operate, is environmentally protective, prepares the polymerization rate uniform and stable of Sodium Polyacrylate, and product obtained has good viscosity, good water solubility, the low, function admirable of residual single amount.
Description
Technical field
The present invention relates to the field of polymers, especially a kind of method that Sodium Polyacrylate is prepared by ternary initiator system.
Background technique
Polyacrylic acid sodium polymerization belongs to typical free radical polymerization, the performance of resulting polyacrylic acid and the chain of polymer
Long, molecular size range and distribution, molecular structure such as linear chain structure or branched structure are related.Sodium Polyacrylate as thickener is wanted
It asks and guarantees under the premise of good aqueous solubility, have enough macromolecules, molecular chain length to provide good toughness, with
Branched structure is reduced, conversion ratio is improved, reduces residual single amount.During sodium acrylate polymerization, Sodium Polyacrylate molecular chain length
It is inversely proportional with the concentration square root of initiator, and its kinetic chain length is proportional to average molecular weight or average degree of polymerization, therefore
The activity and dosage of initiator are most important to the performance of product in the course of the polymerization process.If higher using decomposition activation energy
Initiator, i.e., it is active lower, or be added initiator amount it is very few, the active site that will lead to monomer polymerization is few, that is, generates
Free radical reduce, can not only polymerization rate be made to slow down, monomer is difficult to polymerize completely, conversion ratio reduce, the residual list of product
Amount increases, but also polymer molecular weight can be made to increase, and molecular weight distribution is uneven, or even partial cross-linking, disproportionation occurs, thus
Performance is made it dissolve to decline to a great extent.Still further aspect, if using the lower initiator of decomposition activation energy, i.e., it is active biggish to draw
Hair agent, or the amount of addition initiator are excessive, and the active site that will lead to polymerization reaction increases, that is, the free radical generated increases,
More chain rupture molecular compound is formed, causes molecular weight relatively low.Even, since free radical increases, polymerization rate becomes faster, and
Many polymerization reactions include that the polymerization of sodium acrylate is all exothermic reaction, and the phase can be such that system temperature increases after the reaction, cause to draw
It sends out agent to decompose, generates more free radicals and further result in reaction aggravation, so that polymerization reaction is difficult to control.Preceding late phase reaction temperature
Degree difference leads to reaction speed difference, eventually leads to the polymer molecular weight difference obtained, has a very wide distribution, to make product
It can decline.
The shortcomings that in order to overcome this single initiator to bring, can be such that system causes by stages using composite initiator
Polymerization, this not only makes to react easily controllable, moreover it is possible to obtain the product of superior performance.However it is mainly used about composite initiator at present
In the preparation of polyacrylamide, and there is no effective method for how to prepare Sodium Polyacrylate using composite initiator.Therefore
The method for developing and using composite initiator prepares very that it is necessary to resulting so that polymerization speed is steady for Sodium Polyacrylate
Sodium Polyacrylate even molecular weight distribution, function admirable.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide one kind prepares polypropylene by ternary initiator system
The method of sour sodium.The present invention constitutes ternary initiator system using three kinds of low temperature, medium temperature, high temperature initiators, causes polyacrylic acid
Sodium polymerization passes through the excellent Sodium Polyacrylate of suitable process conditions processability.
The invention adopts the following technical scheme:
A method of Sodium Polyacrylate is prepared by ternary initiator system, comprising the following steps:
(1) by weight, 100 parts of acrylic acid are added in 80-100 parts of distilled water, lye is added dropwise while cooling
140-185 parts, obtain neutralizer；
(2) then by weight filtering neutralizer sequentially adds 5-12.5 parts of medium temperature initiator, high temperature in filtrate
1 part of initiator, 1% 1-3 parts of stannous citrate acid sodium, 4.5-7.5 parts of low temperature initiators, stir evenly, obtain mixed liquor；
(3) mixed liquor reacts 4h at 25-30 DEG C, then dries, and obtains product.
Preferably, cooling described in step (1) is carried out by water-bath, and temperature is no more than 40 during obtaining neutralizer
℃。
Preferably, the lye is the NaOH of 30%-32%, adjusts pH to 8-12.
Preferably, active carbon progress is filtered through described in the step (2).
Preferably, V-50 and 0.1%VA-044 that the medium temperature initiator is 0.1%.
Preferably, the weight ratio of 0.1% V-50 and 0.1%VA-044 is 2.5-7.5:2.5-5.
Preferably, the K that the high-temperature initiator is 0.1%2S2O8。
Preferably, the low temperature initiators are the Na of 0.1-0.3%2S2O8With 0.1% Na2SO3。
Preferably, the Na of the 0.1-0.3%2S2O8With 0.1% Na2SO3Weight ratio be 3-5:1.5-3.3.
The Sodium Polyacrylate obtained by stating method.
Beneficial effects of the present invention
(1) step of the invention is simple, easy to operate, can pass through the initiation reaction that disposably feeds；
(2) preparation method of the invention is environmentally protective, using aqueous solution polymerization, avoids solvent and brings pollution to environment；
(3) present invention prepares the polymerization rate uniform and stable of Sodium Polyacrylate, product good water solubility obtained, residual list
It measures low.
Specific embodiment
Below by embodiment, the present invention will be described in detail.
Embodiment 1
A method of Sodium Polyacrylate is prepared by ternary initiator system, comprising the following steps:
(1) by weight, 100 parts of acrylic acid are added in 100 parts of distilled water, are added dropwise 30% in water-bath cooling
185 parts of NaOH solution, obtain neutralizer；
(2) neutralizer is filtered by active carbon and then by weight sequentially adds 0.1% V-50 5 in filtrate
Part, 0.1% 5 parts of VA-044,0.1% K2S2O81 part, 1% 1 part of stannous citrate acid sodium, 0.3% Na2S2O8
3.3 parts, 0.1% Na2SO3It 3.3 parts, stirs evenly, obtains mixed liquor；
(3) mixed liquor reacts 4h at 30 DEG C, then dries, and obtains product.
Embodiment 2
A method of Sodium Polyacrylate is prepared by ternary initiator system, comprising the following steps:
(1) by weight, 100 parts of acrylic acid are added in 90 parts of distilled water, are added dropwise 32% in water-bath cooling
157 parts of NaOH solution, obtain neutralizer；
(2) neutralizer, then by weight, 0.1% V-50 sequentially added in filtrate are filtered by active carbon
2.5 parts, 0.1% 2.5 parts of VA-044,0.1% K2S2O81 part, 1% 3 parts of stannous citrate acid sodium, 0.1%
Na2S2O85 parts, 0.1% Na2SO3It 2.5 parts, stirs evenly, obtains mixed liquor；
(3) mixed liquor reacts 4h in 25 DEG C, then dries, and obtains product.
Embodiment 3
A method of Sodium Polyacrylate is prepared by ternary initiator system, comprising the following steps:
(1) by weight, 100 parts of acrylic acid are added in 80 parts of distilled water, are added dropwise 32% in water-bath cooling
140 parts of NaOH solution, obtain neutralizer；
(2) neutralizer, then by weight, 0.1% V-50 sequentially added in filtrate are filtered by active carbon
7.5 parts, 0.1% 5 parts of VA-044,0.1% K2S2O81 part, 1% 2 parts of stannous citrate acid sodium, 0.1% Na2S2O8
3 parts, 0.1% Na2SO3It 1.5 parts, stirs evenly, obtains mixed liquor；
(3) mixed liquor reacts 4h in 25 DEG C, then dries, and obtains product.
Experimental example 1
The product that embodiment 1-3 is obtained is compared with existing similar product, test result is as shown in table 1:
The test of 1 properties of product of table
As shown in Table 1, the viscosity for the product that the present invention is prepared is higher than existing similar product, good water solubility, residual
Single amount is low, and showing the present invention, to prepare Sodium Polyacrylate with good performance.
Claims (10)
1. a kind of method for preparing Sodium Polyacrylate by ternary initiator system, which comprises the following steps:
(1) by weight, 100 parts of acrylic acid are added in 80-100 parts of distilled water, lye 140-185 is added dropwise while cooling
Part, obtain neutralizer；
(2) neutralizer is filtered, then by weight, 5-12.5 parts of medium temperature initiator is sequentially added in filtrate, high temperature causes
1 part of agent, 1% 1-3 parts of stannous citrate acid sodium, 4.5-7.5 parts of low temperature initiators, stir evenly, obtain mixed liquor；
(3) mixed liquor reacts 4h at 25-30 DEG C, then dries, and obtains product.
2. being obtained the method according to claim 1, wherein cooling described in step (1) is carried out by water-bath
It is no more than 40 DEG C with temperature during liquid.
3. the method according to claim 1, wherein the lye is the NaOH of 30%-32%.
4. the method according to claim 1, wherein being filtered through active carbon progress described in step (2).
5. the method according to claim 1, wherein the V-50 and 0.1% that the medium temperature initiator is 0.1%
VA-044。
6. according to the method described in claim 5, it is characterized in that, the weight of 0.1% V-50 and 0.1%VA-044
Than for 2.5-7.5:2.5-5.
7. the method according to claim 1, wherein the K that the high-temperature initiator is 0.1%2S2O8。
8. the method according to claim 1, wherein the low temperature initiators are the Na of 0.1-0.3%2S2O8
With 0.1% Na2SO3。
9. according to the method described in claim 8, it is characterized in that, the Na of the 0.1-0.3%2S2O8With 0.1%
Na2SO3Weight ratio be 3-5:1.5-3.3.
10. the Sodium Polyacrylate that any one of claim 1-9 the method obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811261868.1A CN109369833A (en) | 2018-10-26 | 2018-10-26 | A method of Sodium Polyacrylate is prepared by ternary initiator system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811261868.1A CN109369833A (en) | 2018-10-26 | 2018-10-26 | A method of Sodium Polyacrylate is prepared by ternary initiator system |
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| CN109369833A true CN109369833A (en) | 2019-02-22 |
Family
ID=65390052
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|---|---|---|---|
| CN201811261868.1A Pending CN109369833A (en) | 2018-10-26 | 2018-10-26 | A method of Sodium Polyacrylate is prepared by ternary initiator system |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04218502A (en) * | 1990-12-12 | 1992-08-10 | Mitsubishi Petrochem Co Ltd | Production of water-absorbable composite material |
| CN102212241A (en) * | 2011-04-12 | 2011-10-12 | 袁伯才 | Preparation method for acrylate blended emulsion with low residual monomer content |
| CN103242468A (en) * | 2013-04-15 | 2013-08-14 | 北京恒聚化工集团有限责任公司 | Beaded sodium polyacrylate and preparation method thereof |
| CN104628932A (en) * | 2015-02-03 | 2015-05-20 | 江西岳峰高分子材料有限公司 | Initiation system for producing acrylic polymer and application method of initiation system |
-
2018
- 2018-10-26 CN CN201811261868.1A patent/CN109369833A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04218502A (en) * | 1990-12-12 | 1992-08-10 | Mitsubishi Petrochem Co Ltd | Production of water-absorbable composite material |
| CN102212241A (en) * | 2011-04-12 | 2011-10-12 | 袁伯才 | Preparation method for acrylate blended emulsion with low residual monomer content |
| CN103242468A (en) * | 2013-04-15 | 2013-08-14 | 北京恒聚化工集团有限责任公司 | Beaded sodium polyacrylate and preparation method thereof |
| CN104628932A (en) * | 2015-02-03 | 2015-05-20 | 江西岳峰高分子材料有限公司 | Initiation system for producing acrylic polymer and application method of initiation system |
Non-Patent Citations (4)
| Title |
|---|
| 唐蜀忠 等: "自由基聚合氧化还原引发体系的分解速率常数", 《西南石油学院学报》 * |
| 徐坚 等: "《高性能纤维基本科学原理》", 31 July 2018, 国防工业出版社 * |
| 梁璀 等: "复合引发体系制备聚丙烯酸钠", 《安徽化工》 * |
| 王善琦: "《高分子化学原理》", 31 January 1993, 北京航空航天大学出版社 * |
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