CN116178599A - Micro-reaction synthesis method of low molecular weight polyacrylic acid - Google Patents
Micro-reaction synthesis method of low molecular weight polyacrylic acid Download PDFInfo
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- CN116178599A CN116178599A CN202211721709.1A CN202211721709A CN116178599A CN 116178599 A CN116178599 A CN 116178599A CN 202211721709 A CN202211721709 A CN 202211721709A CN 116178599 A CN116178599 A CN 116178599A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 41
- 229920002125 Sokalan® Polymers 0.000 title claims abstract description 24
- 239000004584 polyacrylic acid Substances 0.000 title claims abstract description 24
- 238000001308 synthesis method Methods 0.000 title claims abstract description 16
- 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 28
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- 239000003112 inhibitor Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 6
- 229920000642 polymer Polymers 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 claims description 2
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 2
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 2
- 229950000688 phenothiazine Drugs 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- -1 tetramethyl piperidinol nitroxide radical Chemical class 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 238000009826 distribution Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000005457 ice water Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- 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
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
Abstract
The invention discloses a micro-reaction synthesis method of low molecular weight polyacrylic acid, belonging to the technical field of water treatment. The method comprises the following steps: and (3) reacting the acrylic acid solution, the initiator solution and the polymerization inhibitor solution in a micro-channel reactor synthesis device to obtain a series of low-molecular-weight polyacrylic acid products with the number average molecular weight of 800-5000 and the polymer dispersity index of less than 1.5. The invention adopts the micro-channel reactor synthesis device to realize the synthesis of the acrylic acid oligomer with controllable molecular weight, strengthens the mixing, mass transfer and heat transfer processes in the polymerization reaction process, greatly shortens the reaction time and improves the polymerization efficiency.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a micro-reaction synthesis method of low-molecular-weight polyacrylic acid.
Background
The polyacrylic acid product is a scale inhibiting dispersant commonly used for water treatment, and the annual usage amount of the polyacrylic acid product in China is more than 30 hundred million yuan. As a water treatment agent, domestic and foreign researches prove that the smaller the molecular weight and the narrower the distribution of polyacrylic acid, the stronger the scale inhibition performance of polyacrylic acid. The molecular weight of polyacrylic acid obtained by the free radical polymerization preparation process commonly adopted in China at present is basically more than 2000, and the problems of wide molecular weight distribution, insufficient purity, unstable quality and the like exist. Meanwhile, the traditional synthesis process adopts an intermittent reaction kettle mode for production, and because the traditional stirring kettle is generally lower in mixing and heat exchange performance of a high polymer solution, the concentration distribution of acrylic acid is easy to be uneven in the reaction process, local hot spots are generated, the reaction system is further out of control, an automatic acceleration effect and even bursting aggregation occur, the equipment processing capacity is finally low, the molecular weight distribution of the product is wide, the batch stability is poor, and the performance of polyacrylic acid products is greatly limited.
The same polymer directly determines the advantages and disadvantages of the product and the use safety due to the factors of the molecular weight, the molecular weight distribution, the monomer residue, the byproduct content and the like of the product, and also directly determines the value of the product, so that the controllable preparation process of the low-molecular-weight polyacrylic acid is developed, and the performance of the existing product can be effectively improved.
Disclosure of Invention
The polymerization reaction places high demands on heat transfer and mixing of the reactor, and the drawbacks of conventional tank reactors in this respect become one of the bottlenecks in obtaining high-performance polymerization products. The invention provides a micro-reaction synthesis method of low molecular weight polyacrylic acid, which can prepare a series of low molecular weight polyacrylic acid products with the number average molecular weight of 800-5000g/mol and the polymer dispersity index of less than 1.5.
The aim of the invention is achieved by the following technical scheme:
the invention provides a micro-reaction synthesis method of low molecular weight polyacrylic acid, which comprises the following steps: reacting an acrylic acid solution, an initiator solution and a polymerization inhibitor solution in a micro-channel reactor synthesis device to obtain a series of low-molecular-weight polyacrylic acid products with the number average molecular weight of 800-5000g/mol and the polymer dispersity index of less than 1.5; wherein the initiator is used at a concentration of 5-50% of the mass of the acrylic acid; the polymerization inhibitor is used in an amount of 1-10% of the mass of the initiator; the microchannel reactor synthesis device comprises a microchannel reactor group (1) and a back pressure valve (2) which are connected in series; a metering pump feeding system (3) and a heat conducting oil temperature control system (4) are arranged; each microchannel reactor is provided with two feed inlets and one discharge outlet; the reaction residence time of the reaction in the synthesis device of the microchannel reactor is 0.1-60s, and the reaction temperature is 90-140 ℃.
In the micro-reaction synthesis method, the pore diameter of the channel reactor group is preferably square or round, the effective inner diameter is 200-2000 mu m, and the channels are internally provided with oval internal mixing channels with different numbers; the microchannel length of a single microchannel reactor is 0.5-2.0m.
In the micro-reaction synthesis method, the micro-channel reactor group is preferably formed by combining 2-6 micro-channel reactors in series.
In the micro-reaction synthesis method, the acrylic acid solution comprises, by weight, 20-100% of acrylic acid, 0-80% of water and 0-40% of isopropanol; the initiator solution comprises 4-40% of initiator and 60-96% of water according to weight percentage; the polymerization inhibitor solution comprises 5-10% of polymerization inhibitor and the balance of water according to weight percentage. Further preferably, the mass ratio of the acrylic acid solution to the initiator solution is 1:1.
In the micro-reaction synthesis method, the initiator is ammonium persulfate or potassium persulfate; the polymerization inhibitor is hydroquinone, tetramethyl piperidinol nitroxide radical or p-hydroxyanisole or phenothiazine.
The micro-reaction synthesis method of the low molecular weight polyacrylic acid has the advantages and positive effects that:
1. the process flow is simple, and continuous production can be realized;
2. the reaction time is short, the mass transfer and heat transfer rate is high, and the energy consumption is low;
3. the safety risk is low, the controllability is strong, and the amplification effect is small.
Drawings
FIG. 1 is a schematic diagram of the structure of a synthesis apparatus of a microchannel reactor according to the present invention.
Wherein, 1 is a micro-channel reactor group, 2 is a back pressure valve, 3 is a metering pump feeding system, and 4 is a temperature control system.
Detailed Description
The technical scheme of the invention is further described below by combining specific embodiments. The description of the embodiments of the present invention is merely for illustrating the technical solution of the present invention, and should not limit the scope of the technical solution claimed in the present invention.
Example 1:
the microchannel reactor synthesis apparatus shown in FIG. 1 was used, comprising 6 microchannel reactors connected in series. The specification of a single microchannel reactor is as follows: the inner diameter of the channel is 2000 mu m, the length of the micro-channel is 0.8m, and the liquid holdup is 30mL; the acrylic acid solution (A) comprises, by weight, 60% of acrylic acid, 20% of water and 20% of isopropanol, and the initiator solution (B) comprises, by weight, 16% of ammonium persulfate and 84% of water. The flow rates of A and B are 90mL/min, A and B are injected from two inlets of the 1 st micro-channel reactor simultaneously, the materials at the outlet of the sixth micro-channel reactor are discharged, and ice water bath cooling is performed immediately after discharging. The reaction temperature was set as follows: the 1 st microchannel reactor was not heated, the 2 nd, 3 rd and 4 th microchannel reactors were heated to 115℃and the 5 th and 6 th microchannel reactors were not heated. The residence time of the material from station 1 to station 6 was 60s. The back pressure was set at 0.2MPa.
The reaction results are: polyacrylic acid molecular weight mn=4360 g/mol, pdi=1.29, acrylic acid conversion 99.3%.
Example 2
The microchannel reactor synthesis device shown in fig. 1 comprises a microchannel reactor group formed by connecting 3 microchannel reactors in series. The specification of a single microchannel reactor is as follows: the inner diameter of the channel is 1000 mu m, the length of the micro-channel is 0.7m, and the liquid holdup is 6mL; the acrylic acid solution (A) comprises 60% of acrylic acid and 40% of isopropanol in percentage by weight, and the initiator solution (B) comprises 3% of ammonium persulfate and 97% of water in percentage by weight. The flow rates of A and B are 36mL/min, and the residence time of the materials from the 1 st station to the 3 rd station is 15s; both A and B are injected from two inlets of the 1 st micro-channel reactor, the materials at the outlet of the 3 rd micro-channel reactor are discharged, and the ice water bath is cooled immediately after the materials are discharged. The reaction temperature was set as follows: the 1 st microchannel reactor was not heated, and the 2 nd and 3 rd microchannel reactors were heated to 120 ℃. The back pressure was set at 0.3MPa.
The reaction results are: polyacrylic acid molecular weight mn=4185 g/mol, pdi=1.41, acrylic acid conversion 99.1%.
Example 3
The microchannel reactor synthesis device shown in fig. 1 comprises a microchannel reactor group formed by connecting two microchannel reactors in series. The specification of a single microchannel reactor is as follows: the inner diameter of the channel is 200 mu m, the length of the micro-channel is 2.0m, and the liquid holdup is 1mL; the acrylic acid solution (A) comprises 20% of acrylic acid and 80% of isopropanol in percentage by weight, and the initiator solution (B) comprises 10% of ammonium persulfate and 90% of water in percentage by weight. The flow rates of A and B are 60mL/min, and the residence time of the materials from the 1 st station to the 2 nd station is 1s; both A and B are injected from two inlets of the 1 st micro-channel reactor, the materials at the outlet of the 2 nd micro-channel reactor are discharged, and the ice water bath is cooled immediately after the materials are discharged. The reaction temperature was set as follows: both were heated to 140 c simultaneously. The back pressure was set at 0.6MPa.
The reaction results are: polyacrylic acid molecular weight mn=855 g/mol, pdi=1.12, acrylic acid conversion 98.5%.
Example 4
The microchannel reactor synthesis device shown in fig. 1 comprises a microchannel reactor group formed by connecting 3 microchannel reactors in series. The specification of a single machine is as follows: the inner diameter of the channel is 1600 mu m, the length of the micro-channel is 0.5m, and the liquid holdup is 12mL; the acrylic acid solution (A) comprises 100% of acrylic acid by weight percent, the initiator solution (B) comprises 40% of ammonium persulfate by weight percent and 60% of water by weight percent, the polymerization inhibitor solution (C) comprises 10% of polymerization inhibitor 701 by weight percent, and the balance is water by weight percent. The flow rates of A and B are 180mL/min, the flow rate of C is 90mL/min, and the retention time of materials in the 1 st microchannel reactor and the 2 nd microchannel reactor is 4s; both A and B are injected from two inlets of the 1 st micro-channel reactor, discharged from an outlet of the 3 rd micro-channel reactor, and a polymerization inhibitor solution is injected from one inlet of the 3 rd micro-channel reactor. And cooling in a water bath immediately after discharging. The reaction temperature was set as follows: stations 1 and 2 were heated to 120℃simultaneously. The back pressure was set at 0.3MPa.
The reaction results are: polyacrylic acid molecular weight mn=1296 g/mol, pdi=1.20, acrylic acid conversion 99.2%.
Example 5
The microchannel reactor synthesis device shown in fig. 1 comprises a microchannel reactor group formed by connecting 3 microchannel reactors in series. The specification of a single machine is as follows: the inner diameter of the channel is 1600 mu m, the length of the micro-channel is 0.5m, and the liquid holdup is 12mL; the acrylic acid solution (A) comprises, by weight, 80% of acrylic acid and 20% of water, the initiator solution (B) comprises, by weight, 16% of ammonium persulfate and 84% of water, the polymerization inhibitor solution (C) comprises, by weight, 5% of hydroquinone and the balance of water. The flow rates of A and B are 60mL/min, and the flow rate of C is 30mL/min; the residence time of the materials in the 1 st microchannel reactor and the 2 nd microchannel reactor is 12s, both A and B are injected simultaneously from two inlets of the 1 st microchannel reactor, the materials are discharged from an outlet of the 3 rd microchannel reactor, and one inlet of the 3 rd microchannel reactor is injected with C. And cooling in a water bath immediately after discharging. The reaction temperature was set as follows: stations 1 and 2 were heated to 90 c simultaneously. The back pressure was set at 0.1MPa.
The reaction results are: polyacrylic acid molecular weight mn=2267 g/mol, pdi=1.20, acrylic acid conversion 99.0%.
Claims (6)
1. A micro-reaction synthesis method of low molecular weight polyacrylic acid is characterized in that: reacting an acrylic acid solution, an initiator solution and a polymerization inhibitor solution in a micro-channel reactor synthesis device to obtain a series of low-molecular-weight polyacrylic acid products with the number average molecular weight of 800-5000g/mol and the polymer dispersity index of less than 1.5; wherein the initiator is used at a concentration of 5-50% of the mass of the acrylic acid; the polymerization inhibitor is used in an amount of 1-10% of the mass of the initiator; the microchannel reactor synthesis device comprises a microchannel reactor group (1) and a back pressure valve (2) which are connected in series; a metering pump feeding system (3) and a heat conducting oil temperature control system (4) are arranged; each microchannel reactor is provided with two feed inlets and one discharge outlet; the reaction residence time of the reaction in the synthesis device of the microchannel reactor is 0.1-60s, and the reaction temperature is 90-140 ℃.
2. The micro-reaction synthesis method according to claim 1, wherein: the aperture of the micro-channel reactor group is square or round, the effective inner diameter is 200-2000 mu m, and the channels are provided with oval internal mixing channels with different numbers; the microchannel length of a single microchannel reactor is 0.5-2.0m.
3. The micro-reaction synthesis method according to claim 1, wherein: the micro-channel reactor group is formed by combining 2-6 micro-channel reactors in series.
4. The micro-reaction synthesis method according to claim 1, wherein: the acrylic acid solution comprises, by weight, 20-100% of acrylic acid, 0-80% of water and 0-40% of isopropanol; the initiator solution comprises 4-40% of initiator and 60-96% of water according to weight percentage; the polymerization inhibitor solution comprises 5-10% of polymerization inhibitor and the balance of water according to weight percentage.
5. The micro-reaction synthesis method according to claim 1, wherein: the initiator is ammonium persulfate or potassium persulfate; the polymerization inhibitor is hydroquinone, tetramethyl piperidinol nitroxide radical or p-hydroxyanisole or phenothiazine.
6. The method for synthesizing a micro-reaction according to claim 4, wherein: the mass ratio of the acrylic acid solution to the initiator solution is 1:1.
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| CN202211721709.1A CN116178599A (en) | 2022-12-30 | 2022-12-30 | Micro-reaction synthesis method of low molecular weight polyacrylic acid |
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| CN202211721709.1A CN116178599A (en) | 2022-12-30 | 2022-12-30 | Micro-reaction synthesis method of low molecular weight polyacrylic acid |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110054071A1 (en) * | 2008-05-02 | 2011-03-03 | Basf Se | Method and device for the continuous production of polymers by radical polymerization |
| CN104334589A (en) * | 2012-04-04 | 2015-02-04 | 罗地亚经营管理公司 | Method for synthesising polymers from acrylic acid, one of the salts of same or the mixture thereof |
| CN105273113A (en) * | 2015-10-29 | 2016-01-27 | 清华大学 | Polyacrylic acid synthesis reaction apparatus and polyacrylic acid synthesis method |
| CN114437268A (en) * | 2021-11-17 | 2022-05-06 | 济宁明升新材料有限公司 | Dispersing agent and preparation method thereof |
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- 2022-12-30 CN CN202211721709.1A patent/CN116178599A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110054071A1 (en) * | 2008-05-02 | 2011-03-03 | Basf Se | Method and device for the continuous production of polymers by radical polymerization |
| CN104334589A (en) * | 2012-04-04 | 2015-02-04 | 罗地亚经营管理公司 | Method for synthesising polymers from acrylic acid, one of the salts of same or the mixture thereof |
| CN105273113A (en) * | 2015-10-29 | 2016-01-27 | 清华大学 | Polyacrylic acid synthesis reaction apparatus and polyacrylic acid synthesis method |
| CN114437268A (en) * | 2021-11-17 | 2022-05-06 | 济宁明升新材料有限公司 | Dispersing agent and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 宋顺刚;顾雪萍;王嘉骏;冯连芳;: "微反应器在聚合反应中的应用", 化工进展 * |
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