CN106368061B - A kind of efficient surface sizing agent and preparation method thereof - Google Patents
A kind of efficient surface sizing agent and preparation method thereof Download PDFInfo
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- CN106368061B CN106368061B CN201610746733.9A CN201610746733A CN106368061B CN 106368061 B CN106368061 B CN 106368061B CN 201610746733 A CN201610746733 A CN 201610746733A CN 106368061 B CN106368061 B CN 106368061B
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- monomer
- sizing agent
- preparation
- surface sizing
- acrylate
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Classifications
-
- 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
- C08F212/00—Copolymers 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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- 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
- C08F212/00—Copolymers 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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/12—Monomers containing a branched unsaturated aliphatic radical or a ring substituted by an alkyl radical
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/20—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention discloses a kind of preparation method of efficient surface sizing agent, comprise the following steps：Step 1, methyl styrene, acrylic ester monomer, cross-linking monomer, cationic monomer and initiator are well mixed and form mix monomer；Step 2, the mix monomer obtained is added in 10 20% step 1 in four-hole boiling flask, be warming up to 80 140 DEG C, remaining mix monomer is added dropwise after 5 20 minutes in reaction, and then 80 140 DEG C are incubated 0.5 1.5 hours；Step 3, acetic acid is added, 80 140 DEG C are reacted 20 60 minutes；Step 4, the deionized water of 80 100 DEG C of preheatings is added, continue reaction 0.5 2 hours, cooled down, filtering, obtain efficient surface sizing agent.Cobb values, energy rapid aging can be not only greatly reduced in the efficient surface sizing agent of the present invention, and substantially lower machine is just ripe, and the surface that paperboard body paper can be increased substantially in the case where sizing agent dosage is constant is strong.
Description
Technical field
The present invention relates to technical field of chemical synthesis, more particularly to a kind of preparation method of efficient surface sizing agent.
Background technology
Paper, particularly corrugated paper, the development trend of paperboard are shown：
1）Just develop from high grammes per square metre to low grammes per square metre direction.
2）Wood pulp is replaced using waste paper, but it is high into the intensity difference of paper, hygroscopicity value.
3）The paper quality caused by internal sizing variable factor is more is unstable, class be difficult improve the problem of,
So that manufacturer uses or abandoned less internal sizing, the technique made up using top sizing turns into fashion trend.
Sizing agent requirement for above-mentioned top sizing：A) ring crush intensity is improved；B) Cobb values are greatly reduced（Hygroscopicity value）；
C) it is fast to cure speed, it is desirable to which lower machine is with regard to ripe.
But though present Cypres can improve the certain ring crush intensity of corrugated paper, sizing agent dosage is big, into
This height.
A kind of sizing agent disclosed in Chinese patent CN201210136214.2, although curing speed is fast, and do not get damp,
Be for corrugated paper ring crush intensity improve it is little.
The content of the invention
A kind of efficient surface sizing agent that the present invention proposes for solution above mentioned problem of the prior art and preparation method thereof,
Cobb values, energy rapid aging can be not only greatly reduced in the Cypres, and substantially lower machine is just ripe, and can be in sizing agent dosage
The surface that paperboard body paper is increased substantially in the case of constant is strong.
In order to realize above-mentioned technical purpose, the technical measures that the present invention is taken are：
A kind of preparation method of efficient surface sizing agent, comprises the following steps：
Step 1, methyl styrene, acrylic ester monomer, cross-linking monomer, cationic monomer and initiator are mixed equal
Even formation mix monomer；
Step 2, the mix monomer obtained is added in 10-20% step 1 in four-hole boiling flask, is warming up to 80-140 DEG C, instead
Remaining mix monomer is added dropwise after answering 5-20 minutes, then 80-140 DEG C of insulation 0.5-1.5 hour；
Step 3, add acetic acid, 80-140 DEG C of reaction 20-60 minute；
Step 4, the deionized water of 80-100 DEG C of preheating is added, continue to react 0.5-2 hours, cool down, filtering, obtain height
Imitate Cypres.
In order to further optimize above-mentioned technical proposal, the technical measures that the present invention is taken also include：
Further, step 1 proportioning of each component into step 4 is：
100 parts of methyl styrene
20~100 parts of acrylic ester monomer
20~100 parts of cationic monomer
0~10 part of cross-linking monomer
0.3~5 part of initiator
2~10 parts of acetic acid
160~1785 parts of deionized water.
Further, the acrylic ester monomer is selected from methyl acrylate, ethyl acrylate, propyl acrylate, propylene
Sour N-butyl, isobutyl acrylate, tert-butyl acrylate, Isooctyl acrylate monomer, methyl methacrylate, methacrylic acid second
Ester, propyl methacrylate, n-BMA, Isobutyl methacrylate, Tert-butyl Methacrylate, metering system
At least one of different monooctyl ester of acid.
Further, the cationic monomer is selected from acrylic acid-N, TMSDMA N dimethylamine base ethyl ester and Methacrylamide propyl group
At least one of dimethyl amine.
Further, the cross-linking monomer is selected from hydroxypropyl acrylate, Methacrylamide, acrylamide, N- methylols
Acrylamide, double acrylic acid glycol esters, divinylbenzene, glycidyl acrylate, GMA, N-
Fourth oxygen methacrylic acid, acrylate, acrylic-amino propyl ester, dimethyl m-isopropenyl phenyl isocyanate, first
At least one of base acrylic acid propyl-methyl-diethoxy siloxanes.
Further, the initiator is selected from dibenzoyl peroxide, peroxidized t-butyl perbenzoate, the bay of peroxidating two
At least one of acyl, peroxidating -2- ethyl acid tert-butyl esters.
On the other hand, the present invention provides the efficient surface sizing agent prepared according to above-mentioned preparation method.
Further, the solid content of the Cypres is 15~45wt%.
Further, the pH value of the Cypres is 1-6.
Another further aspect, the present invention also provide application of the above-mentioned efficient surface sizing agent in body paper surface treatment.
The present invention uses above-mentioned technical proposal, compared with prior art, has the following technical effect that：
In the preparation method of the efficient surface sizing agent of the present invention, using the Cypres of self-emulsifying technique preparation, energy
The surface strength while Cobb values for increasing substantially paperboard body paper are also decreased obviously.This may be due to not having in this system
The use of emulsifying agent, reduce the hydrophily of sizing agent, while the crosslinking of some is added in the system of Cypres
Monomer also can be on substantial amounts of with fiber surface hydroxyl and starch molecule hydroxy combining, improve film forming water-resistance and film it is strong
Degree.The surface strength and Cobb values for showing as paper are all improved.The Cypres of the present invention are that one kind can meet paper
The high-performance of top sizing, the product of environmental protection.The product carries out top sizing together with starch to paperboard body paper, can not only change
The Cobb values of kind paperboard, accelerate curing speed, and the surface strength of corrugated paper can be increased substantially.
Embodiment
The invention provides a kind of preparation method of efficient surface sizing agent, comprise the following steps：
Step 1, methyl styrene, acrylic ester monomer, cross-linking monomer, cationic monomer and initiator are mixed equal
Even formation mix monomer；
Step 2, the mix monomer obtained is added in 10-20% step 1 in four-hole boiling flask, is warming up to 80-140 DEG C, instead
Remaining mix monomer is added dropwise after answering 5-20 minutes, then 80-140 DEG C of insulation 0.5-1.5 hour；
Step 3, add acetic acid, 80-140 DEG C of reaction 20-60 minute；
Step 4, the deionized water of 80-100 DEG C of preheating is added, continue to react 0.5-2 hours, cool down, filtering, obtain height
Imitate Cypres.
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1
The preparation of Cypres：
A）By 100 grams of styrene, 20 grams of n-butyl acrylates, 20 grams of acrylic acid-N, TMSDMA N dimethylamine base ethyl ester, 0.3 gram of mistake
Oxidation dibenzoyl is well mixed, standby.
B）161.47 grams of deionized waters are warming up to 80 DEG C, it is standby.
C）With condenser, Dropping feeder, agitator, thermometer four-hole boiling flask in, add 10% step A）In it is mixed
Monomer is closed, is warming up to 80 DEG C, step A is added dropwise after 10 minutes in reaction）In remaining mix monomer, time for adding 5 hours, be added dropwise knot
Continue at 80 DEG C insulation 1 hour after beam, add 10 grams of acetic acid, 80 DEG C of reactions add step B after 1 hour）Hot water, reaction 1
Hour, 35 DEG C are cooled to, pH=1.09.Filtered through 100 mesh filter screens, obtained Cypres, solid content 44.89wt%.
Embodiment 2
The preparation of Cypres：
A）By 100 grams of methyl styrenes, 100 grams of Isooctyl acrylate monomers, 100 grams of dimethylaminopropyl methacrylamides,
10 grams of acrylates, 5 grams of peroxidized t-butyl perbenzoates are well mixed, standby.
B）1783 grams of deionized waters are warming up to 100 DEG C, it is standby.
C）With condenser, Dropping feeder, agitator, thermometer four-hole boiling flask in, add 20% step A）In it is mixed
Monomer is closed, is warming up to 140 DEG C, is added, step A is added dropwise after 10 minutes in reaction）In remaining mix monomer, time for adding 1 hour,
Continue at 140 DEG C insulation 0.5 hour after completion of dropwise addition, add 2 grams of acetic acid, 140 DEG C of reactions add step B after 20 minutes）'s
Hot water, it is cooled to 95 DEG C and reacts 30 minutes, be cooled to 25 DEG C, pH=5.85.Filtered through 100 mesh filter screens, obtained top sizing
Agent, solid content 15.13wt%.
Embodiment 3
The preparation of Cypres：
A）By 100 grams of methyl styrenes, 60 grams of EMAs, 50 grams of dimethylaminopropyl methacrylamides, 5
Gram glycidyl acrylate, 3 grams of peroxidating -2- ethyl acid tert-butyl esters are well mixed, standby.
B）503.7 grams of deionized waters are warming up to 100 DEG C, it is standby.
C）With condenser, Dropping feeder, agitator, thermometer four-hole boiling flask in, add 15% step A）In it is mixed
Monomer is closed, is warming up to 110 DEG C, is added, step A is added dropwise after 10 minutes in reaction）In remaining mix monomer, time for adding 2 hours,
Continue at 110 DEG C insulation 1 hour after completion of dropwise addition, add 5 grams of acetic acid, 110 DEG C of reactions add step B after 40 minutes）Heat
Water, it is cooled to 95 DEG C and reacts 1 hour, be cooled to 25 DEG C, pH=3.58.Filtered through 100 mesh filter screens, obtained Cypres, Gu
Content 30.10wt%.
Embodiment 4
The preparation of Cypres：
A）By 50 grams of methyl styrenes, 50 grams of styrene, 20 grams of Isobutyl methacrylates, 20 grams of methyl methacrylates
Ester, 30 grams of dimethylaminopropyl methacrylamides, 50 grams of acrylic acid-N, TMSDMA N dimethylamine base ethyl ester, 1 gram of divinylbenzene, 2 grams
Dilauroyl peroxide is well mixed, standby.
B）662 grams of deionized waters are warming up to 100 DEG C, it is standby.
C）With condenser, Dropping feeder, agitator, thermometer four-hole boiling flask in, add 15% step A）In it is mixed
Monomer is closed, is warming up to 100 DEG C, is added, step A is added dropwise after 10 minutes in reaction）In remaining mix monomer, time for adding 3 hours,
Continue at 100 DEG C insulation 1 hour after completion of dropwise addition, add 7 grams of acetic acid, 100 DEG C of reactions add step B after 30 minutes）Heat
Water, it is cooled to 95 DEG C and reacts 2 hours, be cooled to 25 DEG C, pH=2.78.Filtered through 100 mesh filter screens, obtained Cypres, Gu
Content 25.21wt%.
Contrast experiment and index determining
It is glued in white card body paper upper surface：
Comparative example：The sizing agent prepared by Chinese patent CN201210136214.2 methods, solid content 15wt%
Sizing agent prepared by the formula of embodiment 1~4,15wt% is diluted to deionized water
The preparation of glue application solution：500 grams of 10wt% oxidized starch aqueous solution are prepared, are warming up to 90 DEG C, are gelatinized 20 minutes, cooling
To 40 DEG C, the sizing agent that comparative example is prepared with the formula of embodiment 1~5 is added（Oxidized starch（It is dry）：Sizing agent（It is wet）=50：
4）, add water and be diluted to 8wt%.
Cobb values determine：
GB/T 1540- suddenly can be pressed by absorbability analyzer using the XSH types of Hangzhou Qingtong Boke Automation Technology Co., Ltd.
1989 methods detect pattern to be measured.
Surface strength determines：
Printed using J-IGT350 types IGT and adapt to instrument measure.
It is glued in white card body paper upper surface：
The glue application solution prepared using comparative example and the formula of embodiment 1~4 is entered on 170 grams of white card body papers with 10# spreading rods
Row coating, coating weight 1.8g/m2, dries 30 seconds or 120 seconds in 110 DEG C of baking ovens respectively after coating, takes out, is cooled to room temperature and enters
Row measure.
Criterion：Cobb values are the smaller the better, and surface strength is the bigger the better.
Specific comparing result is shown in Table 1.
It can be seen that from above-mentioned application result：The sizing agent prepared using the embodiment of the present invention 1~4, compared with comparative example,
Cobb values can be not only significantly improved, while the surface strength of body paper can be increased substantially.
In the preparation method of the efficient surface sizing agent of the present invention, using the Cypres of self-emulsifying technique preparation, energy
The surface strength while Cobb values for increasing substantially paperboard body paper are also decreased obviously.This may be due to not having in this system
The use of emulsifying agent, reduce the hydrophily of sizing agent, while the crosslinking of some is added in the system of Cypres
Monomer also can be on substantial amounts of with fiber surface hydroxyl and starch molecule hydroxy combining, improve film forming water-resistance and film it is strong
Degree.The surface strength and Cobb values for showing as paper are all improved.The Cypres of the present invention are that one kind can meet paper
The high-performance of top sizing, the product of environmental protection.The product carries out top sizing together with starch to paperboard body paper, can not only change
The Cobb values of kind paperboard, accelerate curing speed, and the surface strength of corrugated paper can be increased substantially.
The specific embodiment of the present invention is described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
Substitute also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (9)
1. a kind of preparation method of efficient surface sizing agent, it is characterised in that comprise the following steps：
Step 1, methyl styrene, acrylic ester monomer, cross-linking monomer, cationic monomer and initiator are well mixed shape
Into mix monomer；
Step 2, the mix monomer obtained is added in 10-20% step 1 in four-hole boiling flask, be warming up to 80-140 DEG C, reaction
Remaining mix monomer is added dropwise after 5-20 minutes, then 80-140 DEG C of insulation 0.5-1.5 hour；
Step 3, add acetic acid, 80-140 DEG C of reaction 20-60 minute；
Step 4, the deionized water of 80-100 DEG C of preheating is added, continue to react 0.5-2 hours, cool down, filtering, obtain efficient table
Surface sizing agent；
Step 1 proportioning of each component into step 4 is：
2. preparation method according to claim 1, it is characterised in that the acrylic ester monomer is selected from acrylic acid first
Ester, ethyl acrylate, propyl acrylate, n-butyl acrylate, isobutyl acrylate, tert-butyl acrylate, Isooctyl acrylate monomer,
Methyl methacrylate, EMA, propyl methacrylate, n-BMA, isobutyl
At least one of ester, Tert-butyl Methacrylate, EHMA.
3. preparation method according to claim 1, it is characterised in that the cationic monomer is selected from acrylic acid-N, N- bis-
At least one of methylamino ethyl ester and dimethylaminopropyl methacrylamide.
4. preparation method according to claim 1, it is characterised in that the cross-linking monomer is selected from hydroxypropyl acrylate, first
Base acrylamide, acrylamide, N hydroxymethyl acrylamide, double acrylic acid glycol esters, divinylbenzene, acrylic acid shrink sweet
Grease, GMA, N- fourth oxygen methacrylic acid, acrylate, acrylic-amino propyl ester, diformazan
At least one of isopropenyl phenyl isocyanate, methacrylic acid propyl-methyl-diethoxy siloxanes between base.
5. preparation method according to claim 1, it is characterised in that the initiator is selected from dibenzoyl peroxide, mistake
Aoxidize at least one of t-butyl perbenzoate, dilauroyl peroxide, peroxidating -2- ethyl acid tert-butyl esters.
6. the efficient surface sizing agent prepared according to preparation method described in claim 1-5 any one.
7. efficient surface sizing agent according to claim 6, it is characterised in that the solid content of the Cypres is 15
~45wt%.
8. efficient surface sizing agent according to claim 6, it is characterised in that the pH value of the Cypres is 1-6.
9. application of the efficient surface sizing agent in body paper surface treatment as described in claim 6-8 any one.
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| CN110485201A (en) * | 2018-05-15 | 2019-11-22 | 上海昶法新材料有限公司 | A kind of lignin Cypres and preparation method thereof |
| CN109537358B (en) * | 2018-11-07 | 2022-07-26 | 上海东升新材料有限公司 | Polymerization dispersant and environment-friendly surface sizing agent prepared by adopting same |
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| US6034181A (en) * | 1995-08-25 | 2000-03-07 | Cytec Technology Corp. | Paper or board treating composition of carboxylated surface size and polyacrylamide |
| CN102011343B (en) * | 2010-06-29 | 2012-07-04 | 上海东升新材料有限公司 | Surface sizing agent for corrugated paper as well as preparation method and application thereof |
| CN102086614B (en) * | 2010-08-25 | 2012-11-14 | 永港伟方（北京）科技股份有限公司 | Surface sizing agent as well as preparation method and application thereof |
| CN105874123A (en) * | 2014-01-10 | 2016-08-17 | 栗田工业株式会社 | Use of zirconium-containing additive compositions |
| CN104153249A (en) * | 2014-08-15 | 2014-11-19 | 上海东升新材料有限公司 | Paper surface sizing agent and preparation method thereof |
| CN104846697A (en) * | 2015-04-24 | 2015-08-19 | 杭州百事特实业股份有限公司 | Cation cross-linked styrene-acrylic surface sizing agent and preparation method thereof |
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Effective date of registration: 20190419 Address after: Room 701-A, 7th floor, No. 388 Tianlin Road, Xuhui District, Shanghai, 2003 Co-patentee after: Zhejiang Bangcheng Chemical Co.,Ltd. Patentee after: Shanghai Dongsheng new material Co., Ltd. Address before: Room 701, 7th floor, No. 388 Tianlin Road, Xuhui District, Shanghai 200030 Patentee before: Shanghai Dongsheng new material Co., Ltd. |