CN114106225A - Dispersant for eliminating amplification effect and preparation method thereof - Google Patents

Dispersant for eliminating amplification effect and preparation method thereof Download PDF

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Publication number
CN114106225A
CN114106225A CN202111556660.4A CN202111556660A CN114106225A CN 114106225 A CN114106225 A CN 114106225A CN 202111556660 A CN202111556660 A CN 202111556660A CN 114106225 A CN114106225 A CN 114106225A
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dispersant
parts
acid
aqueous solution
initiator
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施晓旦
孔祥康
尹东华
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Jining Mingsheng New Material Co ltd
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Jining Mingsheng New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers 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
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/04Acids; Metal salts or ammonium salts thereof
    • C08F120/06Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F112/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F112/02Monomers containing only one unsaturated aliphatic radical
    • C08F112/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F112/14Monomers containing only one unsaturated aliphatic radical containing one ring substituted by hetero atoms or groups containing heteroatoms
    • C08F112/22Oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/44Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Emergency Medicine (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The dispersant for eliminating amplification effect of the present invention comprises: 20-60 parts of a monomer; 0.2-3 parts of an initiator; 0.1-1.5 parts of molecular weight regulator; 1-10 parts of a defoaming agent; 5-15 parts of pH value regulator and a proper amount of water. The invention improves the current production condition by introducing the micro-channel experimental method into the experimental production of the dispersing agent; the micro-channel experimental equipment can ensure the consistency of experimental conditions under different production scales, namely the consistency of mass and heat transfer; the experimental environment and conditions are completely the same, the adverse factors after production scale amplification are eliminated, and compared with the traditional production form, the method has obvious advantages and greater development potential.

Description

Dispersant for eliminating amplification effect and preparation method thereof
Technical Field
The invention relates to the field of dispersant preparation, in particular to a dispersant for eliminating amplification effect and a preparation method thereof.
Background
The dispersant is an important assistant in grinding pigment such as calcium carbonate or filler and dispersing paint, and can improve grinding efficiency, stability of slurry and paint, smoothness, whiteness, printing gloss and other properties of paper. The sodium salt of the polyvinyl acid polymer is widely applied in the field, wherein the low molecular weight sodium polyacrylate water solution becomes a main product in the field with excellent dispersibility. However, from the current experimental and production conditions, the traditional kettle type production is mostly adopted, the mode has many disadvantages, especially in the process from small test in a laboratory to pilot test and large production, because the factors such as equipment conversion, material usage increase and the like cause the difference in the amplification process, many good experimental schemes can only stay in the small test stage in the laboratory, industrialization cannot be realized, and the method is a loss for laboratory personnel and society.
The micro-channel experimental method is an experimental method which is researched more in recent years, and on one hand, the micro-channel experimental method has many advantages, such as high mass and heat transfer efficiency; on the other hand, the micro-channel experimental method can ensure the consistency of experimental conditions when the production scale is enlarged, realize undifferentiated enlargement, eliminate various problems generated when the production is enlarged in the traditional mode, and ensure the quality of products.
Disclosure of Invention
The invention aims to provide a dispersant for eliminating amplification effect and a preparation method thereof aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a dispersant for eliminating amplification effect, which comprises the following components in parts by weight:
Figure BDA0003418954480000011
Figure BDA0003418954480000021
preferably, the monomer is selected from at least one of acrylic acid, methacrylic acid, maleic acid, p-styrene sulfonic acid, p-styrene formic acid or p-styrene acetic acid.
Preferably, the initiator is selected from at least one of dibenzoyl peroxide, tert-butyl peroxybenzoate, dilauryl peroxide, butyl hydroperoxide, di-tert-butyl peroxide, dibenzoyl peroxide, azobisisobutyronitrile, ammonia persulfate, sodium persulfate, potassium persulfate, or hydrogen peroxide.
Preferably, the molecular weight regulator is selected from at least one of sodium bisulfite, sodium hypophosphite, sodium metabisulfite, mercaptoethanol, thioglycolic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid or sodium dodecyl sulfonate.
Preferably, the antifoaming agent is selected from at least one of fatty acid ester, fatty amide, aliphatic hydrocarbon, phenethyl alcohol oleate or lauryl phenylacetate.
Preferably, the pH adjuster is selected from at least one of sodium hydroxide, ammonium hydroxide, or potassium hydroxide.
The second aspect of the present invention provides a method for preparing the above dispersant, comprising the steps of:
s1, sequentially weighing 0.2-3 parts of initiator, 0.1-1.5 parts of molecular weight regulator, 1-10 parts of defoamer and 20-60 parts of monomer, and respectively preparing the initiator, the molecular weight regulator and the defoamer into aqueous solutions;
s2, starting equipment, and heating the equipment; after the temperature of the equipment is raised to the reaction temperature, respectively conveying the aqueous solution of the initiator, the aqueous solution of the molecular weight regulator, the aqueous solution of the defoaming agent and the monomer to a microchannel reaction module for reaction; after the reaction time is over, outputting a product from an outlet;
s3, adding a pH value regulator into the product obtained in the step S2, adjusting the pH value to be neutral, and adjusting the solid content to obtain the dispersing agent.
Preferably, in step S1, the initiator is formulated into an aqueous solution with a concentration of 20 wt% to 25 wt%; the concentration of the aqueous solution prepared from the molecular weight regulator is 10-15 wt%; the concentration of the aqueous solution prepared by the defoaming agent is 30-40 wt%.
Preferably, in step S2, the reaction temperature is 70 ℃ to 80 ℃; the reaction time is 5min-15 min.
Preferably, in step S3, the concentration of the pH adjustor is 36 wt% to 45 wt%.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the dispersant for eliminating amplification effect and the preparation method thereof improve the current production condition by introducing the micro-channel experimental method into the experimental production of the dispersant; the micro-channel experimental equipment can ensure the consistency of experimental conditions under different production scales, namely the consistency of mass and heat transfer; the experimental environment and conditions are completely the same, the adverse factors after production scale amplification are eliminated, and compared with the traditional production form, the method has obvious advantages and greater development potential.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1
The embodiment provides a preparation method of a dispersant for eliminating amplification effect, which comprises the following steps:
s1, sequentially weighing 4g of sodium persulfate, 2g of sodium dodecyl sulfate, 20g of phenethyl alcohol oleate and 80g of acrylic acid, and preparing the sodium persulfate, the sodium dodecyl sulfate and the phenethyl alcohol oleate into aqueous solutions respectively;
s2, starting equipment, and heating the equipment; after the temperature of the equipment is raised to 75 ℃, respectively conveying the aqueous solution (with the concentration of 20 wt%) of sodium persulfate, the aqueous solution (with the concentration of 12 wt%) of sodium dodecyl sulfate, the aqueous solution (with the concentration of 30 wt%) of phenethyl alcohol oleate and the acrylic acid to a microchannel reaction module for reaction; after reacting for 5min, outputting a product from an outlet;
s3, adding a sodium hydroxide solution (with the concentration of 36 wt%) into the product obtained in the step S2, adjusting the pH to 6.98 and adjusting the solid content to 40% to obtain the dispersing agent.
The experimental conditions same as the above steps are ensured, 3 groups of reaction modules are added, the material quantity is also enlarged by 3 times, and the above steps are repeated to prepare the dispersing agent again.
The dispersant prepared twice is detected, and the detection results are as follows: viscosity of 230 mPas; the pH was 6.98; the appearance is light yellow transparent viscous liquid.
The results show that: after the production is expanded, products with consistent indexes can be obtained, obvious differences cannot be seen from the appearance and the indexes of the products, the whole experiment process is not subjected to complex debugging, only the experiment module is simply added, and the experiment amplification can be easily carried out by adopting the technology.
Example 2
This example provides another method for preparing a dispersant to eliminate amplification effects, comprising the steps of:
s1, sequentially weighing 2.4g of dilauryl peroxide, 1.2g of sodium hypophosphite, 12g of fatty acid ester and 60g of p-styrene formic acid, and respectively preparing the dilauryl peroxide, the sodium hypophosphite and the fatty acid ester into aqueous solutions;
s2, starting equipment, and heating the equipment; after the temperature of the device is raised to 72 ℃, respectively conveying the aqueous solution of dilauryl peroxide (with the concentration of 25 wt%), the aqueous solution of sodium hypophosphite (with the concentration of 14 wt%), the aqueous solution of fatty acid ester (with the concentration of 35 wt%) and the p-styrene formic acid to a microchannel reaction module for reaction; after reacting for 8min, outputting a product from an outlet;
s3, adding a potassium hydroxide solution (with the concentration of 40 wt%) into the product obtained in the step S2, adjusting the pH to 7.08 and adjusting the solid content to 40% to obtain the dispersing agent.
The experimental conditions same as the above steps are ensured, 5 groups of reaction modules are added, the material quantity is also enlarged by 5 times, and the above steps are repeated to prepare the dispersing agent again.
The dispersant prepared twice is detected, and the detection results are as follows: a viscosity of 237 mPas; the pH was 7.08; the appearance is light yellow transparent viscous liquid.
The results show that: after the production is expanded, products with consistent indexes can be obtained, obvious differences cannot be seen from the appearance and the indexes of the products, the whole experiment process is not subjected to complex debugging, only the experiment module is simply added, and the experiment amplification can be easily carried out by adopting the technology.
In conclusion, the dispersant for eliminating the amplification effect and the preparation method thereof improve the current production condition by introducing the micro-channel experimental method into the experimental production of the dispersant; the micro-channel experimental equipment can ensure the consistency of experimental conditions under different production scales, namely the consistency of mass and heat transfer; the experimental environment and conditions are completely the same, the adverse factors after production scale amplification are eliminated, and compared with the traditional production form, the method has obvious advantages and greater development potential.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.

Claims (10)

1. A dispersant for eliminating amplification effect is characterized by comprising the following components in parts by weight:
Figure FDA0003418954470000011
2. the dispersant of claim 1, wherein said monomer is selected from at least one of acrylic acid, methacrylic acid, maleic acid, p-styrenesulfonic acid, p-styreneformic acid, or p-styreneacetic acid.
3. The dispersant of claim 1, wherein said initiator is selected from at least one of dibenzoyl peroxide, t-butyl peroxybenzoate, dilauryl peroxide, butyl hydroperoxide, ditert-butyl peroxide, dibenzoyl peroxide, azobisisobutyronitrile, ammonia persulfate, sodium persulfate, potassium persulfate, or hydrogen peroxide.
4. The dispersant of claim 1, wherein the molecular weight modifier is selected from at least one of sodium bisulfite, sodium hypophosphite, sodium metabisulfite, mercaptoethanol, thioglycolic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid, or sodium dodecyl sulfate.
5. The dispersant of claim 1, wherein the defoamer is selected from at least one of a fatty acid ester, a fatty amide, an aliphatic hydrocarbon, a phenethyl alcohol oleate, or a lauryl phenylacetate.
6. The dispersant of claim 1, wherein the pH adjuster is at least one selected from the group consisting of sodium hydroxide, ammonium hydroxide, and potassium hydroxide.
7. A method of preparing the dispersant of claims 1-6, comprising the steps of:
s1, sequentially weighing 0.2-3 parts of initiator, 0.1-1.5 parts of molecular weight regulator, 1-10 parts of defoamer and 20-60 parts of monomer, and respectively preparing the initiator, the molecular weight regulator and the defoamer into aqueous solutions;
s2, starting equipment, and heating the equipment; after the temperature of the equipment is raised to the reaction temperature, respectively conveying the aqueous solution of the initiator, the aqueous solution of the molecular weight regulator, the aqueous solution of the defoaming agent and the monomer to a microchannel reaction module for reaction; after the reaction time is over, outputting a product from an outlet;
s3, adding a pH value regulator into the product obtained in the step S2, adjusting the pH value to be neutral, and adjusting the solid content to obtain the dispersing agent.
8. The method according to claim 7, wherein in step S1, the initiator is formulated into an aqueous solution with a concentration of 20 wt% to 25 wt%; the concentration of the aqueous solution prepared from the molecular weight regulator is 10-15 wt%; the concentration of the aqueous solution prepared by the defoaming agent is 30-40 wt%.
9. The method according to claim 7, wherein, in step S2, the reaction temperature is 70 ℃ to 80 ℃; the reaction time is 5min-15 min.
10. The method according to claim 7, wherein the concentration of the pH adjustor is 36 wt% to 45 wt% in step S3.
CN202111556660.4A 2021-12-17 2021-12-17 Dispersant for eliminating amplification effect and preparation method thereof Pending CN114106225A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008239967A (en) * 2007-02-27 2008-10-09 Sekisui Plastics Co Ltd Method for producing acrylic resin particle and method for producing resin particle
CN101781378A (en) * 2010-02-25 2010-07-21 寿光德圣造纸化工有限公司 Method for preparing ammonium-sodium polyacrylate dispersant
CN105273113A (en) * 2015-10-29 2016-01-27 清华大学 Polyacrylic acid synthesis reaction apparatus and polyacrylic acid synthesis method
CN111206453A (en) * 2020-02-26 2020-05-29 济宁明升新材料有限公司 Efficient composite dispersant and preparation method thereof
CN112920325A (en) * 2021-01-28 2021-06-08 南京桥健高分子材料有限公司 Dispersing agent and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008239967A (en) * 2007-02-27 2008-10-09 Sekisui Plastics Co Ltd Method for producing acrylic resin particle and method for producing resin particle
CN101781378A (en) * 2010-02-25 2010-07-21 寿光德圣造纸化工有限公司 Method for preparing ammonium-sodium polyacrylate dispersant
CN105273113A (en) * 2015-10-29 2016-01-27 清华大学 Polyacrylic acid synthesis reaction apparatus and polyacrylic acid synthesis method
CN111206453A (en) * 2020-02-26 2020-05-29 济宁明升新材料有限公司 Efficient composite dispersant and preparation method thereof
CN112920325A (en) * 2021-01-28 2021-06-08 南京桥健高分子材料有限公司 Dispersing agent and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
姚忠平等: "《药用高分子材料学》", 哈尔滨工业大学出版社, pages: 134 *
张龙等: "《绿色化学(第二版)》", 31 August 2014, 华中科技大学出版社, pages: 358 - 359 *

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