CN106223116B - A kind of Cypres and preparation method thereof - Google Patents
A kind of Cypres and preparation method thereof Download PDFInfo
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- CN106223116B CN106223116B CN201610745869.8A CN201610745869A CN106223116B CN 106223116 B CN106223116 B CN 106223116B CN 201610745869 A CN201610745869 A CN 201610745869A CN 106223116 B CN106223116 B CN 106223116B
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- cypres
- monomer
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- acrylate
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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
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/66—Salts, e.g. alums
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of preparation method of Cypres, comprise the following steps：Step 1, methyl styrene, acrylic ester monomer, cationic monomer and initiator are well mixed and form mix monomer；Step 2, the mix monomer obtained is added in 10% 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, after being cooled to 25 35 DEG C, added zirconates, stir, filter, obtain Cypres.Cobb values, energy rapid aging can be not only greatly reduced in the Cypres of the present invention, and substantially lower machine is just ripe, and the surface strength of body paper can be significantly put forward in the case where sizing agent dosage is constant.
Description
Technical field
The present invention relates to technical field of chemical synthesis, more particularly to a kind of Cypres and preparation method thereof.
Background technology
Paper, particularly corrugated paper, paperboard development trend and it is related the problem of show：
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,
Improved less for the ring crush intensity of corrugated paper.
The content of the invention
A kind of preparation method for Cypres that the present invention proposes for solution above mentioned problem of the prior art so that system
Cobb values, energy rapid aging can be not only greatly reduced in standby Cypres, and substantially lower machine is just ripe, and can be used in sizing agent
Measure it is constant in the case of significantly put forward the surface strength of body paper.
In order to realize above-mentioned technical purpose, the technical measures that the present invention is taken are：
A kind of preparation method of Cypres, it is characterised in that comprise the following steps：
Step 1, methyl styrene, acrylic ester monomer, cationic monomer and initiator are well mixed and form mixing
Monomer；
Step 2, the mix monomer obtained is added in 10% 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, after being cooled to 25-35 DEG C,
Zirconates is added, is stirred, filters, obtains Cypres.
In order to further optimize above-mentioned technical proposal, the technical measures that the present invention is taken also include：
Preferably, 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 zirconates
0.3~5 part of initiator
2~10 parts of acetic acid
160~1785 parts of deionized water.
Preferably, the acrylic ester monomer is selected from methyl acrylate, ethyl acrylate, propyl acrylate, acrylic acid
N-butyl, isobutyl acrylate, tert-butyl acrylate, Isooctyl acrylate monomer, methyl methacrylate, EMA,
Propyl methacrylate, n-BMA, Isobutyl methacrylate, Tert-butyl Methacrylate, methacrylic acid
At least one of different monooctyl ester.
Preferably, the cationic monomer is selected from acrylic acid-N, TMSDMA N dimethylamine base ethyl ester and Methacrylamide propyl group two
At least one of methyl amine.
Preferably, the zirconates is selected from least one of zirconium carbonate, acetic acid zirconium.
Preferably, 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 also provides surface prepared by 7. preparation methods according to claim 1-6 any one
Sizing agent.
Preferably, the solid content of the Cypres is 15~45wt%.
Preferably, the pH value of the Cypres is 1-6.
Another further aspect, the present invention also provide application of the above-mentioned Cypres 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 Cypres of the present invention, the inventors discovered that adding a small amount of zirconium in Cypres
Salt, it is unexpected, the surface strength of body paper can be increased substantially while the Cobb values of body paper have also declined.This may be due to
Zirconates can improve the active force between fiber fines with the substantial amounts of hydroxy combining of fiber surface, make the fibre compact degree of paper
Improve.Meanwhile strengthen the crosslinking degree of starch during applying glue, improve the water-resistance of film forming and reach reduction Cobb values, improve surface
The effect of intensity.Cypres prepared by the present invention are a kind of high-performance that can meet paper for surface sizing, the production of environmental protection
Product.The Cypres prepared using the present invention carry out top sizing together with starch to body paper, can not only improve body paper
Cobb values, accelerate curing speed, and the surface strength of body paper can be increased substantially.
Embodiment
The invention provides a kind of preparation method of Cypres, it is characterised in that comprises the following steps：
Step 1, methyl styrene, acrylic ester monomer, cationic monomer and initiator are well mixed and form mixing
Monomer；
Step 2, the mix monomer obtained is added in 10% 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, after being cooled to 25-35 DEG C,
Zirconates is added, is stirred, filters, obtains 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=1.13.Filtered through 100 mesh filter screens, obtained Cypres, solid content 44.93wt%.
Embodiment 2
The preparation of Cypres：
A）By 100 grams of methyl styrenes, 100 grams of Isooctyl acrylate monomers, 100 grams of dimethylaminopropyl methacrylamides, 5
Gram peroxidized t-butyl perbenzoate is 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, add 10 grams of zirconium carbonates, stir, pH=5.98.Through 100 mesh
Strainer filtering, obtained Cypres, solid content 15.23wt%.
Embodiment 3
The preparation of Cypres：
A）By 100 grams of methyl styrenes, 60 grams of EMAs, 50 grams of dimethylaminopropyl methacrylamides, 3
Gram peroxidating -2- ethyl acid the 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, add 5 grams of acetic acid zirconiums, stir, pH=3.68.Through 100 mesh filter screens
Filtering, obtained Cypres, solid content 30.13wt%.
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, 2 grams of bays of peroxidating two
Acyl 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, add 0.5 gram of acetic acid zirconium, 0.5 gram of zirconium carbonate, stir, pH=
2.54.Filtered through 100 mesh filter screens, obtained Cypres, solid content 25.10wt%.
The Comparison study of embodiment and comparative example
It is glued in xerography 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 xerography body paper upper surface：
The glue application solution prepared using comparative example and the formula of embodiment 1~4 uses 10# spreading rods on 70 grams of xerography body paper
It is coated, coating weight 1.8g/m2, is dried 30 seconds or 120 seconds in 110 DEG C of baking ovens respectively after coating, takes out, be cooled to room temperature
It is measured.
Criterion：Cobb values are the smaller the better, and surface strength is the bigger the better.Cobb values and surface strength situation are 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 Cypres of the present invention, the inventors discovered that adding a small amount of zirconium in Cypres
Salt, it is unexpected, the surface strength of body paper can be increased substantially while the Cobb values of body paper have also declined.This may be due to
Zirconates can improve the active force between fiber fines with the substantial amounts of hydroxy combining of fiber surface, make the fibre compact degree of paper
Improve.Meanwhile strengthen the crosslinking degree of starch during applying glue, improve the water-resistance of film forming and reach reduction Cobb values, improve surface
The effect of intensity.Cypres prepared by the present invention are a kind of high-performance that can meet paper for surface sizing, the production of environmental protection
Product.The Cypres prepared using the present invention carry out top sizing together with starch to body paper, can not only improve body paper
Cobb values, accelerate curing speed, and the surface strength of body 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 Cypres, it is characterised in that comprise the following steps：
Step 1, well mixed formed of methyl styrene, acrylic ester monomer, cationic monomer and initiator is mixed into list
Body；
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, after being cooled to 25-35 DEG C, added
Zirconates, stir, filter, obtain Cypres；
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 zirconates in zirconium carbonate, acetic acid zirconium extremely
Few one kind.
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 Cypres prepared according to preparation method described in claim 1-5 any one.
7. Cypres according to claim 6, it is characterised in that the solid content of the Cypres be 15~
45wt%.
8. Cypres according to claim 6, it is characterised in that the pH value of the Cypres is 1-6.
9. application of the Cypres in body paper surface treatment as described in claim 6-8 any one.
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| CN201610745869.8A CN106223116B (en) | 2016-08-29 | 2016-08-29 | A kind of Cypres and preparation method thereof |
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| CN201610745869.8A CN106223116B (en) | 2016-08-29 | 2016-08-29 | A kind of Cypres and preparation method thereof |
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| CN106967194A (en) * | 2017-04-20 | 2017-07-21 | 上海东升新材料有限公司 | A kind of wallpaper styrene-acrylic latex |
| CN107033275A (en) * | 2017-04-20 | 2017-08-11 | 上海东升新材料有限公司 | A kind of wallpaper styrene-acrylic latex and preparation method thereof |
| CN106977663A (en) * | 2017-04-20 | 2017-07-25 | 上海东升新材料有限公司 | A kind of special styrene-acrylic latex of wallpaper |
| CN113150202A (en) * | 2021-05-10 | 2021-07-23 | 华东理工大学 | Preparation method of surface sizing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5824190A (en) * | 1995-08-25 | 1998-10-20 | Cytec Technology Corp. | Methods and agents for improving paper printability and strength |
| CN101806019B (en) * | 2010-04-01 | 2011-12-28 | 宁夏茂弘浆纸化学品有限公司 | Surface sizing agent for papermaking and production process thereof |
| 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 |
| EP3092339A1 (en) * | 2014-01-10 | 2016-11-16 | Kurita Water Industries Ltd. | Use of zirconium-containing additive compositions |
| 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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