CN110485201A - A kind of lignin Cypres and preparation method thereof - Google Patents
A kind of lignin Cypres and preparation method thereof Download PDFInfo
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- CN110485201A CN110485201A CN201810460931.8A CN201810460931A CN110485201A CN 110485201 A CN110485201 A CN 110485201A CN 201810460931 A CN201810460931 A CN 201810460931A CN 110485201 A CN110485201 A CN 110485201A
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- lignin
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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
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Abstract
It is the aqueous dispersion as made of the copolymerization of lignin, alkali, trimethylamine, epoxychloropropane, acid, cross-linking monomer, (methyl) acrylic ester monomer, (methyl) styrene and initiator the invention discloses a kind of lignin Cypres.Lignin Cypres of the invention are the products of a kind of high-performance for being able to satisfy paper for surface sizing, environmental protection.The product carries out top sizing to fluting medium together with starch, can not only improve the Cobb value of corrugated paper, accelerates curing speed, and can increase substantially the surface ring crush intensity of corrugated paper, adapts to the needs of highly intensified corrugated paper development.The lignin generated in paper-making process can be used as starting material in the Cypres simultaneously, significantly reduces production cost.
Description
Technical field
The present invention relates to paper surface-sizing agent fields, and in particular to a kind of lignin Cypres and its preparation side
Method.
Background technique
Paper, especially corrugated paper, paperboard development trend 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 at the intensity difference of paper, hygroscopicity value is high.
3) internal sizing variable factor it is more caused by paper quality is unstable, class is difficult the problem of improving,
So that manufacturer uses or abandon less internal sizing, fashion trend is become using the technique that top sizing is made up.It applies on surface
The addition of jelly can improve page characteristic or increase surface property, intensity and the water-resistance of Paper or cardboard.
Sizing agent requirement for above-mentioned top sizing: ring crush intensity a) is improved；B) Cobb value (hygroscopicity value) is greatly reduced；
C) curing speed is fast, it is desirable that 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, at
This height.
A kind of sizing agent disclosed in Chinese patent CN107034730A, although rate of drying is fast, for corrugated paper
Ring crush intensity improves little.
Summary of the invention
The object of the present invention is to provide a kind of lignin Cypres and preparation method thereof, to solve background technique presence
Drawbacks described above.
The present invention realizes by the following technical solutions:
A kind of lignin Cypres, be by lignin, alkali, trimethylamine, epoxychloropropane, acid, cross-linking monomer,
Aqueous dispersion made of (methyl) acrylic ester monomer, (methyl) styrene and initiator copolymerization.
Further, the parts by weight of each component are as follows:
The alkali generally selects inorganic base, preferably at least one of sodium hydroxide, potassium hydroxide and ammonium hydroxide.
The acid can be organic acid or inorganic acid, preferably at least one of hydrochloric acid, acetic acid and sulfuric acid.
(methyl) acrylic ester monomer is being selected from methyl acrylate, ethyl acrylate, propyl acrylate, acrylic acid just
Butyl ester, isobutyl acrylate, tert-butyl acrylate, Isooctyl acrylate monomer, methyl methacrylate, ethyl methacrylate, first
Base propyl acrylate, n-BMA, Isobutyl methacrylate, Tert-butyl Methacrylate, methacrylic acid are different
At least one of monooctyl ester.
The cross-linking monomer be selected from hydroxypropyl acrylate, Methacrylamide, acrylamide, N hydroxymethyl acrylamide,
Double acrylic acid glycol esters, divinylbenzene, glycidyl acrylate, glycidyl methacrylate, N- fourth oxygen methyl
Acrylic acid, acrylate, acrylic-amino propyl ester, dimethyl m-isopropenyl phenyl isocyanate, methacrylic acid
At least one of propyl-methyl-diethoxy siloxanes.
The initiator is selected from least one of hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, tert-butyl hydroperoxide.
Water in component is as the dispersion solvent in reaction process, and dosage does not have considered critical, those skilled in the art
Member can need suitably to adjust amount of water according to real reaction, and preferred dosage is 150~3060 parts by weight.
Lignin Cypres of the present invention, prepare with the following method:
(methyl) styrene, (methyl) acrylic ester monomer and cross-linking monomer are mixed and are made into mix monomer by step 1；
Initiator is dissolved in suitable quantity of water and is made into initiator solution by step 2；
Lignin, trimethylamine, alkali and suitable quantity of water are added in the reactor, epoxy chloropropionate is added after completely dissolution for step 3
Alkane reaction；
Step 4 continuously adds acid, and the mix monomer is then added simultaneously and initiator solution carries out polymerization reaction,
Obtain the lignin Cypres.
Preferably, the reaction temperature of step 3 is 45-70 DEG C；The reaction temperature of step 4 is 70-95 DEG C.
Lignin Cypres of the present invention, the surface treatment for fluting medium.
The inventors discovered that by carrying out the lignin Cypres that chemical modification obtains to lignin, unexpectedly
, the Cobb value of the ring crush intensity while corrugated paper that can increase substantially corrugated paper is decreased obviously.This may be due in the present invention
In to lignin carry out it is cation-modified during in lignin hydrophilic hydroxyl be shielded, while in cationic polymer
Cation group can be combined by ionic bond, be played with the hydroxy combining of starch in a large amount of hydroxyl of fiber surface and glue application solution
The effect of bridge formation improves the active force between fiber fines and enhances the apparent ring crush intensity of corrugated paper.In addition, in the present invention
Partial cross-linked monomer is added, the bonding action between enhancing starch and fiber can be assisted, improves the airtightness of glue application solution film forming
Can, it improves paper strength, improve paper water suction.
Lignin Cypres of the invention are the productions of a kind of high-performance for being able to satisfy paper for surface sizing, environmental protection
Product.The product carries out top sizing to fluting medium together with starch, can not only improve the Cobb value of corrugated paper, accelerates curing speed
Degree, and the surface ring crush intensity of corrugated paper can be increased substantially, adapt to the needs of highly intensified corrugated paper development.
Specific embodiment
The present invention is illustrated below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1:
A) by 20 grams of styrene, 20 grams of n-butyl acrylates are uniformly mixed, spare.
B) 0.3 gram of ammonium persulfate is dissolved in 10 grams of deionized waters, it is spare.
C) in the four-hole boiling flask for having condenser, Dropping feeder, blender, thermometer, 143.3 grams of deionizations are added
Water, 10 grams of potassium hydroxide, 1 gram of trimethylamine, 100 grams of lignin are warming up to 45 DEG C after being completely dissolved, 1 gram of epoxychloropropane is added dropwise,
Time for adding 0.25 hour.Continue heat preservation 0.75 hour.70 DEG C are warming up to, 1 gram of hydrochloric acid is added.In 70 DEG C of a dropping step A) in
Mix monomer, time for adding 1 hour；Simultaneously a dropping step B) in initiator solution, time for adding 1 hour, after completion of dropwise addition
Continue heat preservation 1 hour at 70 DEG C, is cooled to 25 DEG C, pH=6.23.It is filtered through 100 mesh filter screens, obtained lignin top sizing
Agent, solid content 49.92wt%.
Embodiment 2
A) by 100 grams of methyl styrenes, 100 grams of Isooctyl acrylate monomers, 100 grams of hydroxypropyl acrylates are uniformly mixed, spare.
B) 10 grams of sodium peroxydisulfates are dissolved in 100 grams of deionized waters, it is spare.
C) in the four-hole boiling flask for having condenser, Dropping feeder, blender, thermometer, 2960 grams of deionized waters are added,
40 grams of ammonium hydroxide, 25 grams of trimethylamines, 100 grams of lignin are warming up to 55 DEG C after being completely dissolved, 25 grams of epoxychloropropane are added dropwise,
Time for adding 1 hour.Continue heat preservation 2 hours.95 DEG C are warming up to, 40 grams of sulfuric acid are added.In 95 DEG C of a dropping step A) in mixing
Monomer, time for adding 3 hours；Simultaneously a dropping step B) in initiator solution, time for adding 3 hours, 95 after completion of dropwise addition
DEG C continue heat preservation 2 hours, is cooled to 25 DEG C, pH=1.18.It is filtered through 100 mesh filter screens, obtained lignin Cypres, Gu
Content 15.25wt%.
Embodiment 3
A) by 60 grams of methyl styrenes, 50 grams of ethyl methacrylate, 50 grams of glycidyl methacrylate mixing are
It is even, it is spare.
B) 6 grams of hydrogen peroxide are dissolved in 100 grams of deionized waters, it is spare.
C) in the four-hole boiling flask for having condenser, Dropping feeder, blender, thermometer, 684 grams of deionized waters are added,
20 grams of sodium hydroxides, 15 grams of trimethylamines, 100 grams of lignin are warming up to 65 DEG C after being completely dissolved, 15 grams of epoxychloropropane are added dropwise,
Time for adding 2 hours.Continue heat preservation 1 hour.85 DEG C are warming up to, 20 grams of acetic acid are added.In 85 DEG C of a dropping step A) in mixing
Monomer, time for adding 1.5 hours；Simultaneously a dropping step B) in initiator solution, time for adding 2 hours, after completion of dropwise addition
85 DEG C are continued heat preservation 1 hour, are cooled to 25 DEG C, pH=4.54.It is filtered through 100 mesh filter screens, obtained lignin Cypres,
Solid content 29.68wt%.
Embodiment 4
A) by 10 grams of methyl styrenes, 20 grams of styrene, 20 grams of Isobutyl methacrylates, 20 grams of methyl methacrylates
Ester, 30 grams of acrylates are uniformly mixed, spare.
B) 4 grams of hydrogen peroxide are dissolved in 100 grams of deionized waters, it is spare.
C) in the four-hole boiling flask for having condenser, Dropping feeder, blender, thermometer, 976 grams of deionized waters are added,
25 grams of sodium hydroxides, 10 grams of trimethylamines, 100 grams of lignin are warming up to 70 DEG C after being completely dissolved, 18 grams of epoxychloropropane are added dropwise,
Time for adding 1 hour.Continue heat preservation 1 hour.80 DEG C are warming up to, 12 grams of acetic acid are added.In 80 DEG C of a dropping step A) in mixing
Monomer, time for adding 2 hours；Simultaneously a dropping step B) in initiator solution, time for adding 3 hours, 80 after completion of dropwise addition
DEG C continue heat preservation 1 hour, is cooled to 25 DEG C, pH=5.06.It is filtered through 100 mesh filter screens, obtained lignin Cypres, Gu
Content 20.13wt%.
Embodiment 5
A) by 40 grams of methyl styrenes, 30 grams of styrene, 50 grams of Tert-butyl Methacrylates, 5 grams of propyl methacrylates,
15 grams of dimethyl m-isopropenyl phenyl isocyanates are uniformly mixed, spare.
B) 5 grams of hydrogen peroxide, 2 grams of tert-butyl hydroperoxide are dissolved in 100 grams of deionized waters, it is spare.
C) in the four-hole boiling flask for having condenser, Dropping feeder, blender, thermometer, 383 grams of deionized waters are added,
15 grams of sodium hydroxides, 22 grams of trimethylamines, 100 grams of lignin are warming up to 60 DEG C after being completely dissolved, 13 grams of epoxychloropropane are added dropwise,
Time for adding 1 hour.Continue heat preservation 0.5 hour.90 DEG C are warming up to, 25 grams of hydrochloric acid are added.In 90 DEG C of a dropping step A) in it is mixed
Conjunction monomer, time for adding 2.5 hours；Simultaneously a dropping step B) in initiator solution, time for adding 2.5 hours, completion of dropwise addition
Continue heat preservation 1 hour at 90 DEG C afterwards, is cooled to 25 DEG C, pH=2.87.It is filtered through 100 mesh filter screens, obtained lignin surface is applied
Jelly, solid content 40.10wt%.
Embodiment 6
It is glued in corrugated paper upper surface:
Comparative example: the sizing agent prepared by the method for Chinese patent CN107034730A embodiment 1, solid content are
15wt%.
Sizing agent prepared by Examples 1 to 5 formula is diluted to 15wt% with deionized water.
The preparation of glue application solution: preparing 500 grams of 10wt% oxidized starch aqueous solutions, is warming up to 90 DEG C, is gelatinized 20 minutes, cooling
To 40 DEG C, add comparative example and Examples 1 to 5 formula preparation sizing agent (oxidized starch (dry): sizing agent (wet)=50:
4) it, adds water and is diluted to 8wt%.
The measurement of Cobb value:
GB/T1540- suddenly can be pressed by absorbability analyzer using the XSH type of Hangzhou Qingtong Boke Automation Technology Co., Ltd.
1989 methods detect pattern to be measured.
Ring crush intensity measurement:
Pattern to be measured is detected using the CT300A compressive strength tester of Hangzhou Qingtong Boke Automation Technology Co., Ltd..
It is glued in corrugated paper upper surface:
The glue application solution prepared using comparative example and Examples 1 to 5 formula on 120 grams of fluting mediums with 10# spreading rod into
Row coating, coating weight 2g/m2, dried 30 seconds or 120 seconds in 110 DEG C of baking ovens respectively after coating, take out, be cooled to room temperature progress
Measurement.Criterion: Cobb value is the smaller the better, and ring crush index is the bigger the better.Measurement result is shown in Table 1.
1 product performance index of table
From it is above-mentioned using result it can be seen that using the embodiment of the present invention 1~5 prepare sizing agent, compared with comparative example,
The ring crush intensity of paper can not only be increased substantially, significantly improve Cobb value, while the Cobb value of paper, ring crush index be not after being glued
It is not much different with the curing time, curing speed is fast.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of lignin Cypres, which is characterized in that it is by lignin, alkali, trimethylamine, epoxychloropropane, acid, friendship
Aqueous dispersion made of receipts or other documents in duplicate body, (methyl) acrylic ester monomer, (methyl) styrene and initiator copolymerization.
2. lignin Cypres as described in claim 1, which is characterized in that the parts by weight of each component are as follows:
3. lignin Cypres as described in claim 1, which is characterized in that the alkali is selected from sodium hydroxide, hydroxide
At least one of potassium and ammonium hydroxide.
4. lignin Cypres as described in claim 1, which is characterized in that the acid is selected from hydrochloric acid, acetic acid and sulfuric acid
At least one of.
5. lignin Cypres as described in claim 1, which is characterized in that (methyl) the acrylic ester monomer choosing
From methyl acrylate, ethyl acrylate, propyl acrylate, n-butyl acrylate, isobutyl acrylate, tert-butyl acrylate, third
The different monooctyl ester of olefin(e) acid, methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-BMA, methyl
At least one of isobutyl acrylate, Tert-butyl Methacrylate, isooctyl methacrylate.
6. lignin Cypres as described in claim 1, which is characterized in that the cross-linking monomer is selected from acrylic acid hydroxypropyl
Ester, Methacrylamide, acrylamide, N hydroxymethyl acrylamide, double acrylic acid glycol esters, divinylbenzene, acrylic acid
Ethylene oxidic ester, glycidyl methacrylate, N- fourth oxygen methacrylic acid, acrylate, acrylic-amino third
Ester, dimethyl m-isopropenyl phenyl isocyanate, in methacrylic acid propyl-methyl-diethoxy siloxanes at least
It is a kind of.
7. lignin Cypres as described in claim 1, which is characterized in that the initiator is selected from hydrogen peroxide, mistake
At least one of ammonium sulfate, sodium peroxydisulfate, tert-butyl hydroperoxide.
8. the method for preparing any one of the claim 1-7 lignin Cypres, which is characterized in that including walking as follows
It is rapid:
(methyl) styrene, (methyl) acrylic ester monomer and cross-linking monomer are mixed and are made into mix monomer by step 1；
Initiator is dissolved in suitable quantity of water and is made into initiator solution by step 2；
Lignin, trimethylamine, alkali and suitable quantity of water is added in step 3 in the reactor, and it is anti-that epoxychloropropane is added after completely dissolution
It answers；
Step 4 continuously adds acid, and the mix monomer is then added simultaneously and initiator solution carries out polymerization reaction, obtains
The lignin Cypres.
9. method according to claim 8, which is characterized in that the reaction temperature of step 3 is 45-70 DEG C；The reaction of step 4
Temperature is 70-95 DEG C.
10. the application of any one of the claim 1-7 lignin Cypres, which is characterized in that for fluting medium
Surface treatment.
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