CN109537358B - Polymerization dispersant and environment-friendly surface sizing agent prepared by adopting same - Google Patents
Polymerization dispersant and environment-friendly surface sizing agent prepared by adopting same Download PDFInfo
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- CN109537358B CN109537358B CN201811319187.6A CN201811319187A CN109537358B CN 109537358 B CN109537358 B CN 109537358B CN 201811319187 A CN201811319187 A CN 201811319187A CN 109537358 B CN109537358 B CN 109537358B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
-
- 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
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- 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
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/08—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated side groups
- C08F290/12—Polymers provided for in subclasses C08C or C08F
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/38—Sulfohalogenation
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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)
- General Chemical & Material Sciences (AREA)
- Paper (AREA)
Abstract
The invention discloses a polymeric dispersant, and a preparation method thereof comprises the following steps: mixing maleic anhydride and polyvinyl alcohol, heating to melt, and performing polycondensation reaction; and cooling after the reaction is finished, and adding chlorosulfonic acid until the reaction is completed to obtain the polymeric dispersant. The invention also discloses an environment-friendly surface sizing agent, and the preparation method comprises the following steps: mixing the polymeric dispersant, acetic acid and water, and then adding an initiator for reaction; continuously dropwise adding (methyl) styrene and (methyl) acrylate monomers, and fully reacting to obtain the surface sizing agent. The environment-friendly surface sizing agent is a high-performance and environment-friendly product which can meet the requirement of paper surface sizing. The product and starch are used together for surface sizing of base paper, and the water resistance of paper can be obviously improved. Meanwhile, the polymeric dispersant has better emulsifying property, so that the synthesized emulsion has lower residual monomers.
Description
Technical Field
The invention relates to the field of preparation of surface sizing agents, in particular to an environment-friendly paper surface sizing agent with strong water resistance.
Background
The addition of the surface sizing agent can improve the paper performance or increase the surface performance, strength and water resistance of the paper or the paperboard.
The surface sizing agent has great significance for the development of the paper industry, and paper makers hope to improve the paper performance and the product grade by surface sizing so as to meet the continuous development requirements of the current paper making, printing and related fields. The performance of the surface sizing agent product directly influences the surface sizing effect. The polymer surface sizing agent as a new product appearing in recent years is rapidly developed in the paper industry by the unique performance, can meet the production requirements of various paper products, and provides powerful guarantee for the development of high-grade paper and special paper.
The research and development work of domestic polymer surface sizing agents starts late, products developed at present have certain gaps compared with the product performance of a plurality of foreign chemical companies, and particularly the market of the surface sizing agents of high-grade paper is almost monopolized by the foreign companies. Therefore, research and development of polymer surface sizing agents with wide application range, high efficiency, low price and environmental friendliness are necessary and urgent, and the polymer surface sizing agent has profound significance for improving the paper quality, reducing the production cost of enterprises, replacing foreign imported products, enhancing the competitive power of paper products and promoting the development of the paper industry in China.
In the prior art, a sizing agent disclosed in CN106223116B has a high Cobb value of paper, but the resultant product has a large amount of VOC residue.
Therefore, the development of a method which can effectively reduce the Cobb value of paper and ensure that the synthetic product has lower VOC residue is in line with the development trend of modern chemicals and is one of the key points of current research and development of technical personnel in the field.
Disclosure of Invention
The invention aims to provide a polymeric dispersant and an environment-friendly surface sizing agent prepared by adopting the polymeric dispersant, so as to solve the defects in the prior art.
The invention is realized by the following technical scheme:
the polymeric dispersant is prepared by the polycondensation reaction of maleic anhydride and polyvinyl alcohol and the reaction of the polycondensation product with chlorosulfonic acid.
The preparation method of the polymeric dispersant comprises the following steps: mixing maleic anhydride and polyvinyl alcohol, heating to melt, and performing polycondensation reaction; and cooling after the reaction is finished, and adding chlorosulfonic acid until the reaction is completed to obtain the polymeric dispersant.
Preferably, the use amounts of the components are respectively as follows according to parts by weight:
100 parts of maleic anhydride,
800 portions of 600 portions of polyvinyl alcohol,
Chlorosulfonic acid 120-150 portions.
Preferably, the polycondensation reaction is carried out at the temperature of 80-120 ℃ for 2-4hr, the temperature is reduced to 40-60 ℃ after the reaction is finished, chlorosulfonic acid is added, and the reaction is continued for 1-3hr to obtain the polymeric dispersant.
The invention also provides a preparation method of the environment-friendly surface sizing agent, which comprises the following steps:
step one, mixing the polymeric dispersant, acetic acid and water, heating to 80-90 ℃, and then adding an initiator for reaction;
and step two, continuously dropwise adding (methyl) styrene and (methyl) acrylate monomers, and fully reacting to obtain the surface sizing agent.
As a preferred technical scheme, the use amounts of the components are respectively as follows according to parts by weight:
wherein water is used to disperse the components, the amount of water can be easily adjusted by one skilled in the art according to the actual use requirements of the product. Preferably 450-670 parts. Of course, an appropriate amount of water may be added to the formulation of the present invention to adjust the solid content of the final product, for example, 300-900 parts by weight of water may be added.
Preferably, the (meth) acrylate monomer is at least one selected from the group consisting of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, t-butyl acrylate, isooctyl acrylate, t-butyl methacrylate, isooctyl methacrylate, n-propyl acrylate, cyclohexyl acrylate, lauryl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, and methyl methacrylate.
Preferably, the initiator is at least one selected from dibenzoyl peroxide, tert-butyl peroxybenzoate, dilauryl peroxide, potassium persulfate, ammonium persulfate, hydrogen peroxide, tert-butyl hydroperoxide, sodium persulfate, hydrogen peroxide-ferrous sulfate, sodium persulfate-sodium sulfite, sodium persulfate-sodium bisulfite, and sodium persulfate-sodium hypophosphite.
As a further preferred embodiment, the initiator may be added all at once in step one, or a portion may be added in step one, and then the remaining portion may be added in the polymerization reaction in step two. If the initiator is added in two portions, at least 60% by weight of the total amount of initiator is added in step one.
The environment-friendly surface sizing agent prepared by the invention has the solid content of 25-30 wt% and the pH value of 1-2.
The invention also provides an application of the environment-friendly surface sizing agent in paper surface sizing, and specifically comprises the following steps of mixing the environment-friendly surface sizing agent with gelatinized oxidized starch according to a mass ratio of 0.7-1.2: 100 (both are absolute dry weight) to obtain a sizing solution for sizing the surface of paper.
The environment-friendly surface sizing agent disclosed by the invention can greatly reduce the Cobb value of paper after being coated on the surface of the paper, and meanwhile, when a residual monomer of the surface sizing agent is detected, the residual VOC of the sizing agent is found to be low, so that the environment-friendly requirement of the current government on chemical products is met. The low VOC of the sizing agent is mainly because maleic anhydride is adopted in the polymerization dispersing agent, the maleic anhydride contains double bonds, and when emulsion polymerization is carried out in the second step, the double bonds in the maleic anhydride react with monomers to graft the monomers on the molecules of the polymerization dispersing agent, so that the polymerization dispersing agent has good dispersibility, and the synthesized emulsion only has less free dispersing agent and oligomer. Meanwhile, after the surface sizing agent is coated on the surface of paper after the polymeric dispersant and the monomer are polymerized, the paper has better water resistance, which shows that the Cobb value of the paper is lower.
The environment-friendly surface sizing agent is a high-performance and environment-friendly product which can meet the requirement of paper surface sizing. The product and starch are used together for surface sizing of base paper, so that the water resistance of paper can be obviously improved. Meanwhile, the polymeric dispersant has better emulsifying property, so that the synthesized emulsion has lower residual monomer.
Detailed Description
The invention is illustrated below by means of specific examples, without restricting it.
Example 1
1. Preparation of a polymeric dispersant:
a1000 ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer was charged with 100g of maleic anhydride and 600 g of polyvinyl alcohol, heated and melted, and reacted at 80 ℃ for 3 hr. Cooling to 40 deg.C, adding 120g chlorosulfonic acid, and reacting for 1 hr.
2. Preparation of the environment-friendly surface sizing agent:
in a 1000ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer, 10 g of polymeric dispersant, 500 g of deionized water and 4g of acetic acid were added, and then the temperature was raised to 80 ℃ and 1g of ammonium persulfate was added. After 10min of reaction, 180 g of the mixed monomer (100g of styrene and 80g of ethyl acrylate) was slowly dropped for 1.5 hr. 0.5 g of ammonium persulfate was added and the reaction was continued for 1 hr. After cooling, the surface sizing agent is obtained by filtering through a 325-mesh filter screen, wherein the pH value is 1.28, and the solid content is 27.2%.
Example 2
1. Preparation of a polymeric dispersant:
a1000 ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer was charged with 100g of maleic anhydride and 650 g of polyvinyl alcohol, heated to dissolve them, and reacted at 90 ℃ for 3 hr. Cooling to 50 deg.C, adding 125g chlorosulfonic acid, and reacting for 1.5 hr.
2. Preparation of the environment-friendly surface sizing agent:
in a 1000ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer, 20g of a polymeric dispersant, 600 g of deionized water and 4g of acetic acid were added, and then the temperature was raised to 90 ℃ and 1g of potassium persulfate was added. After 10min of reaction, 200 g of the mixed monomer (100g of styrene and 100g of n-butyl acrylate) was slowly dropped for 2.0 hr. 0.5 g of potassium persulfate was added and the reaction was continued for 1 hr. After cooling, the surface sizing agent is obtained by filtering through a 325-mesh filter screen, wherein the pH value is 1.35, and the solid content is 26.0%.
Example 3
1. Preparation of a polymeric dispersant:
a1000 ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer was charged with 100g of maleic anhydride and 700 g of polyvinyl alcohol, heated to dissolve, and reacted at 95 ℃ for 3 hr. Cooling to 50 deg.C, adding 130g chlorosulfonic acid, and reacting for 2.5 hr.
2. Preparation of environment-friendly surface sizing agent:
in a 1000ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer, 35g of polymeric dispersant, 530 g of deionized water and 4g of acetic acid were added, and then the temperature was raised to 90 ℃ and 3g of dibenzoyl peroxide was added. After 15min of reaction, 160 g of the mixed monomer (100g of styrene and 60g of isooctyl acrylate) was slowly added dropwise over 2.0 hr. 1.0 g of potassium persulfate was added and the reaction was continued for 1 hr. After cooling, the surface sizing agent is obtained by filtering through a 325-mesh filter screen, wherein the pH value is 1.50, and the solid content is 26.5%.
Example 4
1. Preparation of a polymeric dispersant:
a1000 ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer was charged with 100g of maleic anhydride and 700 g of polyvinyl alcohol, heated to dissolve, and reacted at 90 ℃ for 2.5 hr. Cooling to 45 deg.C, adding 130g chlorosulfonic acid, and reacting for 2.0 hr.
2. Preparation of the environment-friendly surface sizing agent:
in a 1000ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer, 30g of polymeric dispersant, 530 g of deionized water and 4g of acetic acid were added, and then the temperature was raised to 85 ℃ and 3g of dibenzoyl peroxide was added. After 15min of reaction, 150 g of the mixed monomer (100g of styrene and 50g of isooctyl acrylate) was slowly added dropwise over 2.5 hr. 1.0 g of potassium persulfate was added and the reaction was continued for 1 hr. After cooling, the surface sizing agent is obtained by filtering through a 325-mesh filter screen, wherein the pH value is 1.42, and the solid content is 25.5%.
Example 5
1. Preparation of a polymeric dispersant:
a1000 ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer was charged with 100g of maleic anhydride and 750 g of polyvinyl alcohol, heated to dissolve, and reacted at 100 ℃ for 3 hr. Cooling to 50 deg.C, adding 135g chlorosulfonic acid, and reacting for 2.5 hr.
2. Preparation of environment-friendly surface sizing agent:
in a 1000ml four-neck flask equipped with a condenser, a dropping device, a stirrer and a thermometer, 40 g of polymeric dispersant, 510 g of deionized water and 4g of acetic acid were added, and then the temperature was raised to 90 ℃ and 3g of t-butyl peroxybenzoate was added. After 15min of reaction, 180 g of the mixed monomer (100g of styrene and 80g of isooctyl acrylate) was slowly added dropwise over 2.0 hr. 1.0 g ammonium persulfate was added and the reaction was continued for 1 hr. After cooling, the surface sizing agent is obtained by filtering through a 325-mesh filter screen, wherein the pH is 1.39, and the solid content is 29.8%.
Comparative example
The sizing agent prepared according to the method of example 4 of chinese patent CN106245431A was used as a comparative example diluted to 15 wt% with deionized water.
Application examples
The environment-friendly surface sizing agent prepared in the examples 1 to 5 is diluted to 15 wt% by deionized water.
Preparation of a sizing solution: preparing 500 g of 10 wt% oxidized starch aqueous solution, heating to 90 ℃, gelatinizing for 20 minutes, cooling to 40 ℃, adding the sizing agent (oxidized starch (dry): sizing agent (wet): 50: 3) prepared by the formula of the comparative example and the examples 1-5, and adding water to dilute to 8 wt%.
Determination of Cobb value:
and detecting the paper sample to be detected by adopting a brisbone absorbency tester according to the GB/T1540-1989 method.
And (3) residual monomer determination:
and testing the surface sizing agent by adopting a gas chromatography-mass spectrometer.
Sizing on the surface of the special paper:
sizing solutions prepared using the formulations of comparative examples and examples 1-5 were used to apply the above sizes to specialty papers at the same size (1.3 g/m per side) on a laboratory mini size press 2 ) Respectively sizing on single side, drying the sized paper sample on a glazing machine at the same temperature and time (150 ℃ 20s), and curing the paper sample for 5min before measurement. The measurement results are shown in Table 1.
TABLE 1 product Performance index
| Sample (I) | Cobb value (g/m) 2 ) | Residual monomer (ppm) |
| Blank space | 105 | / |
| Comparative example | 45 | 3000 |
| Example 1 | 33 | 600 |
| Example 2 | 35 | 550 |
| Example 3 | 30 | 480 |
| Example 4 | 28 | 490 |
| Example 5 | 36 | 520 |
From the above application results, it can be seen that: compared with a comparative example, the surface sizing agent of the invention can not only reduce the Cobb value of paper, but also greatly reduce residual monomers in sizing liquid.
The foregoing shows and describes the general principles, principal features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for preparing a polymeric dispersant, comprising the steps of: mixing maleic anhydride and polyvinyl alcohol, heating to melt, and performing polycondensation reaction; cooling after the reaction is finished, and adding chlorosulfonic acid until the reaction is completed to obtain the polymeric dispersant; the dosage of each component is calculated according to the parts by weight as follows: 100 parts of maleic anhydride, 800 parts of 600-800 parts of polyvinyl alcohol and 150 parts of chlorosulfonic acid; the polycondensation reaction is carried out at 80-120 deg.C for 2-4hr, and then cooled to 40-60 deg.C, chlorosulfonic acid is added, and the reaction is continued for 1-3hr to obtain the polymeric dispersant.
2. The preparation method of the environment-friendly surface sizing agent is characterized by comprising the following steps:
mixing the polymeric dispersant of claim 1, acetic acid and water, and adding an initiator to react;
continuously adding (methyl) styrene and (methyl) acrylate monomers, and fully reacting to obtain the environment-friendly surface sizing agent;
the dosage of each component is calculated according to the parts by weight as follows: 10-50 parts of polymeric dispersant, 100 parts of (methyl) styrene, 40-100 parts of (methyl) acrylate monomer, 0.5-5 parts of initiator, 4-8 parts of acetic acid and a proper amount of water.
3. The method of claim 2, wherein the (meth) acrylate monomer is selected from at least one of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, t-butyl acrylate, isooctyl acrylate, t-butyl methacrylate, isooctyl methacrylate, n-propyl acrylate, cyclohexyl acrylate, lauryl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, and methyl methacrylate.
4. The method of claim 2, wherein the initiator is selected from at least one of dibenzoyl peroxide, t-butyl peroxybenzoate, dilauryl peroxide, potassium persulfate, ammonium persulfate, hydrogen peroxide, t-butyl hydroperoxide, sodium persulfate, hydrogen peroxide-ferrous sulfate, sodium persulfate-sodium sulfite, sodium persulfate-sodium bisulfite, sodium persulfate-sodium hypophosphite.
5. The process according to claim 2, wherein 60% by weight of the total amount of initiator is added in step one and the remainder of the initiator is added in the polymerization reaction in step two.
6. Use of an environment friendly surface sizing agent prepared according to any one of claims 2-5 in surface sizing of paper, characterized in that the environment friendly surface sizing agent is mixed with gelatinized oxidized starch in a mass ratio of 0.7-1.2: 100 to obtain sizing liquid for sizing the surface of paper.
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| CN110409219A (en) * | 2019-07-25 | 2019-11-05 | 上海东升新材料有限公司 | A kind of method of soap-free emulsion method synthetic environment-friendly Cypres |
| CN111533840B (en) * | 2020-06-24 | 2022-02-01 | 浙江恒达新材料股份有限公司 | Environment-friendly water-resistant reinforced latex for paper and preparation method and application thereof |
| CN112626915A (en) * | 2020-12-15 | 2021-04-09 | 上海东升新材料有限公司 | Preparation method and application of high-whiteness paper surface sizing agent |
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| US5438087A (en) * | 1989-12-28 | 1995-08-01 | Japan Pmc Corporation | Paper sizing composition |
| JPH1087745A (en) * | 1996-08-20 | 1998-04-07 | Chevron Chem Co | New ternary copolymer as disperser |
| CN101164956A (en) * | 2007-09-28 | 2008-04-23 | 上海东升新材料有限公司 | Cement disperser and its preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1266567A (en) * | 1969-04-24 | 1972-03-15 | ||
| US20050261142A1 (en) * | 2004-05-18 | 2005-11-24 | The Lubrizol Corporation, A Corporation Of The State Of Ohio | Polymeric dispersant viscosity modifier composition |
| CN100500995C (en) * | 2006-10-11 | 2009-06-17 | 上海东升新材料有限公司 | Sizing agent for treating paper surface and its preparing method and use |
| CN101314930B (en) * | 2008-07-21 | 2012-04-25 | 上海东升新材料有限公司 | Surface sizing agent special for corrugated paper, preparation and application thereof |
| CN102775563B (en) * | 2011-05-10 | 2013-12-25 | 永港伟方（北京）科技股份有限公司 | Dispersing agent, and preparation method and application thereof |
| CN102345246A (en) * | 2011-07-13 | 2012-02-08 | 天津三农金科技有限公司 | Dispersant used for paper pulp |
| CN103554362B (en) * | 2013-10-18 | 2016-03-16 | 中国科学院广州化学研究所 | A kind of copolymer-maleic anhydride dispersion agent and preparation method thereof and application |
| CN106368061B (en) * | 2016-08-29 | 2018-03-13 | 上海东升新材料有限公司 | A kind of efficient surface sizing agent and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5438087A (en) * | 1989-12-28 | 1995-08-01 | Japan Pmc Corporation | Paper sizing composition |
| JPH1087745A (en) * | 1996-08-20 | 1998-04-07 | Chevron Chem Co | New ternary copolymer as disperser |
| CN101164956A (en) * | 2007-09-28 | 2008-04-23 | 上海东升新材料有限公司 | Cement disperser and its preparing method |
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