CN116355115A - Preparation method of high molecular weight sodium polyacrylate - Google Patents
Preparation method of high molecular weight sodium polyacrylate Download PDFInfo
- Publication number
- CN116355115A CN116355115A CN202310120227.9A CN202310120227A CN116355115A CN 116355115 A CN116355115 A CN 116355115A CN 202310120227 A CN202310120227 A CN 202310120227A CN 116355115 A CN116355115 A CN 116355115A
- Authority
- CN
- China
- Prior art keywords
- molecular weight
- high molecular
- sodium polyacrylate
- product
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 title claims abstract description 19
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229940047670 sodium acrylate Drugs 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000018044 dehydration Effects 0.000 claims abstract description 8
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 230000003797 telogen phase Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 7
- 239000010842 industrial wastewater Substances 0.000 abstract description 6
- -1 acrylic ester Chemical class 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000008394 flocculating agent Substances 0.000 abstract description 3
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002455 scale inhibitor 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to the technical field of sodium polyacrylate preparation, and in particular discloses a preparation method of high molecular weight sodium polyacrylate, which comprises the following steps: adding sodium acrylate aqueous solution and an initiator into a reaction kettle, starting stirring, and heating to 65-70 ℃; slowly dripping a telogen at a constant speed to initiate reaction, wherein the adding speed is that the adding is finished within 60-120min, and the adding is continuously heated to 80-90 ℃; preserving heat and reacting for 1-2h; after the reaction, carrying out negative pressure dehydration and concentration until the water content of the product is 20-30%, wherein the dehydration temperature is controlled at 80 ℃; putting the product containing a small amount of water into an oven to be dried for 6 hours at the temperature of 120 ℃; pulverizing the obtained dried product to obtain powder product. The high molecular weight sodium polyacrylate powder product prepared by the invention can play a role of a flocculating agent, can fully recycle industrial wastewater containing sodium acrylate as a main component generated in the production of acrylic ester, and reduces wastewater output.
Description
Technical Field
The invention relates to the technical field of sodium polyacrylate preparation, in particular to a preparation method of high molecular weight sodium polyacrylate.
Background
At present, the molecular weight of the domestic sodium polyacrylate product is mainly 10 4 Hereinafter, they are used as water-dispersing agents and scale inhibitors; in addition, when acrylic ester is produced, industrial wastewater containing sodium acrylate as a main component is produced, and if the industrial wastewater can be recycled, the environmental pollution can be greatly reduced, and the wastewater output can be reduced.
Therefore, how to recycle industrial wastewater is an important link in the current production.
Disclosure of Invention
The invention aims to provide a preparation method of high molecular weight sodium polyacrylate, which not only can realize wastewater utilization, but also can obtain the relative molecular weight of 10 6 -10 7 The high molecular weight sodium polyacrylate is used for the use of flocculant, and increases the application range of the high molecular weight sodium polyacrylate for the recycling of the wastewater containing acrylic acid in workshops.
In order to solve the technical problems, the invention provides a preparation method of high molecular weight sodium polyacrylate, which comprises the following steps:
s1, adding a sodium acrylate aqueous solution and an initiator into a reaction kettle, starting stirring, and heating to 65-70 ℃;
s2, slowly and uniformly dripping a telogen to initiate reaction, and continuously heating to 80-90 ℃ while adding, wherein the adding speed is 60-120min, and the adding is finished;
s3, carrying out heat preservation reaction for 1-2h;
s4, carrying out negative pressure dehydration and concentration until the water content of the product is 20-30% after the reaction is finished, and controlling the dehydration temperature at 80 ℃;
s5, putting the product containing a small amount of water into an oven to be dried for 6 hours at the temperature of 120 ℃;
s6, crushing the obtained dried product to prepare a powdery product.
Further, the concentration of the sodium acrylate aqueous solution in the S1 is 25-30%, the PH value is 5-7, and the initiator accounts for 0.5-1% of the mass ratio of the sodium acrylate aqueous solution.
Furthermore, the telogen in the S2 accounts for 2.5-5% of the mass of the sodium acrylate aqueous solution.
Further, the initiator in the step S1 comprises one or more of ammonium persulfate, potassium persulfate, hydrogen peroxide and the like.
Further, the telogen in S2 includes one or more of isopropanol, sodium sulfite, sodium bisulphite, ferrous sulfate, etc.
The beneficial effects of the invention are as follows:
1. the invention can fully recycle the industrial wastewater containing sodium acrylate as a main component generated in the production of acrylic ester, reduce the output of the wastewater, achieve recycling of recycling economy and increase the application range of the wastewater containing acrylic acid in workshops.
2. The relative molecular weight of the high molecular weight sodium polyacrylate prepared by the invention is 10 6 -10 7 Can be used for the use of flocculating agent, and has wide application prospect and marketization value.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
2000g of sodium acrylate aqueous solution with the concentration of 20 percent and 5g of potassium persulfate are sequentially added into a reaction kettle, stirred and heated to 65 ℃ and then slowly heatedSlowly adding 200g of sodium bisulphite aqueous solution with concentration of 40% at constant speed, finishing the addition at 60 min, raising the reaction temperature to 80-85 ℃, preserving heat and reacting for 2h, vacuum dehydrating until the water content of the product is 30% after the reaction is finished, putting into a baking oven for drying at 120 ℃ for 6h, obtaining solid, crushing into powder product, and measuring the relative molecular mass of the powder product to be 1.6X10 6 。
Example 2:
2000g of sodium acrylate aqueous solution with the concentration of 25 percent and 10g of potassium persulfate are sequentially added into a reaction kettle, stirred and heated to 65 ℃, 200g of sodium bisulphite aqueous solution with the concentration of 40 percent is slowly and uniformly added, the reaction temperature is increased to 80-85 ℃ after 60 min addition is finished, the reaction is carried out for 2 hours while the reaction is carried out, the vacuum dehydration is carried out until the water content of the product is 30 percent after the reaction is finished, the product is put into a baking oven at 120 ℃ and dried for 6 hours, the solid is obtained and crushed into a powder product, and the relative molecular mass of the product is measured to be 3.1 multiplied by 10 6 。
Example 3:
2000g of sodium acrylate aqueous solution with the concentration of 30 percent and 20g of potassium persulfate are sequentially added into a reaction kettle, stirred and heated to 65 ℃, slowly and uniformly added with sodium bisulphite aqueous solution with the concentration of 30 percent, the reaction temperature is increased to 85-90 ℃ after the addition of 60 min, the reaction is carried out for 2 hours while the heat preservation is carried out, the vacuum dehydration is carried out until the water content of the product is 30 percent after the reaction is finished, the product is put into a baking oven for drying at 120 ℃ for 6 hours, the solid is crushed into powder products, and the relative molecular mass of the powder products is measured to be 8.2 multiplied by 10 6 。
The invention can fully recycle the industrial wastewater containing sodium acrylate as a main component generated in the production of acrylic ester, reduce the output of the wastewater, achieve recycling of recycling economy and increase the application range of the wastewater containing acrylic acid in workshops.
And the relative molecular weight of the high molecular weight sodium polyacrylate prepared by the method is 10 6 -10 7 Can be used for the use of flocculating agent, and has wide application prospect and marketization value.
The foregoing disclosure is merely illustrative of the preferred embodiments of the present invention and is not intended to limit the scope of the claims herein, as equivalent changes may be made in the claims herein without departing from the scope of the invention.
Claims (5)
1. A method for preparing high molecular weight sodium polyacrylate, which is characterized by comprising the following steps:
s1, adding a sodium acrylate aqueous solution and an initiator into a reaction kettle, starting stirring, and heating to 65-70 ℃;
s2, slowly and uniformly dripping a telogen to initiate reaction, and continuously heating to 80-90 ℃ while adding, so as to ensure that dripping is finished within 60-120 min;
s3, carrying out heat preservation reaction for 1-2h;
s4, carrying out negative pressure dehydration and concentration until the water content of the product is 20-30% after the reaction is finished, and controlling the dehydration temperature at 80 ℃;
s5, putting the product containing a small amount of water into an oven to be dried for 6 hours at the temperature of 120 ℃;
s6, crushing the obtained dried product to prepare a powdery product.
2. The preparation method of the high molecular weight sodium polyacrylate according to claim 1, wherein the concentration of the sodium acrylate aqueous solution in the S1 is 25-30%, the PH value is 5-7, and the initiator accounts for 0.5-1% of the sodium acrylate aqueous solution by mass.
3. The preparation method of the high molecular weight sodium polyacrylate according to claim 1, wherein the telogen in the S2 accounts for 2.5-5% of the mass of the sodium acrylate aqueous solution.
4. The method for preparing high molecular weight sodium polyacrylate according to claim 1, wherein the initiator in S1 comprises one or more of ammonium persulfate, potassium persulfate, hydrogen peroxide, and the like.
5. The method for preparing high molecular weight sodium polyacrylate according to claim 1, wherein the telogen in S2 comprises one or more of isopropanol, sodium sulfite, sodium bisulphite, ferrous sulfate, etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310120227.9A CN116355115A (en) | 2023-02-16 | 2023-02-16 | Preparation method of high molecular weight sodium polyacrylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310120227.9A CN116355115A (en) | 2023-02-16 | 2023-02-16 | Preparation method of high molecular weight sodium polyacrylate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116355115A true CN116355115A (en) | 2023-06-30 |
Family
ID=86912409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310120227.9A Pending CN116355115A (en) | 2023-02-16 | 2023-02-16 | Preparation method of high molecular weight sodium polyacrylate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116355115A (en) |
-
2023
- 2023-02-16 CN CN202310120227.9A patent/CN116355115A/en active Pending
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |