CN104120626A - A sizing agent, a preparing method thereof and applications of the sizing agent - Google Patents
A sizing agent, a preparing method thereof and applications of the sizing agent Download PDFInfo
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- CN104120626A CN104120626A CN201410328290.2A CN201410328290A CN104120626A CN 104120626 A CN104120626 A CN 104120626A CN 201410328290 A CN201410328290 A CN 201410328290A CN 104120626 A CN104120626 A CN 104120626A
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Abstract
The invention relates to a sizing agent, a preparing method thereof and applications of the sizing agent. The sizing agent is prepared by the following steps of: (1) reacting palmitic acid and diethylenetriamine under existence of a catalyst at 90-180 DEG C for 3-10 h to obtain fatty amide, with the adding mass ratio of the palmitic acid to the diethylenetriamine being 0.1-20:1; (2) adding the fatty amide obtained in the step (1) into a reacting container, adding dimethyl carbonate and sodium hydroxide under stirring with the temperature being controlled to be 50-95 DEG C, the adding mass ratio of the fatty amide to the dimethyl carbonate being 0.05-25:1, and the mass ratio of the fatty amide to the sodium hydroxide being 0.1-30:1; and reacting for 2-7 h after the addition is finished. The sizing agent can be used for adding into pulp and for surface glue sizing. No matter which using manner is adopted, the sizing agent can largely enhance water resistance of paper and enhance surface strength of paper. Paper or paper boards sized with a glue by a glue sizing method provided by the invention is good in water resistance and high in surface strength.
Description
Technical field
The present invention relates to a kind of sizing agent and its preparation method and application.
Background technology
At present, along with improving constantly of scientific and technical fast development and people's living standard, the performance requirement of the paper of people to various difference in functionality is also more and more higher.In order to meet people's application demand, the product quality of oneself just must improve by variety of way in paper plant, such as the WATER RESISTANCE in order to improve paper and surface strength, often adopts the mode of applying glue so that paper performance reaches requirement.The resin application methods of present commonplace use is mainly divided into two kinds: plasm-glue-blending and top sizing.
The mode of adding in slurry is to add sizing agent at the wet end of paper machine, and kind is mainly that neutral and alkali sizing agent is as alkyl ketene dimer (abbreviation AKD), alkenyl succinic anhydride (being called for short ASA) etc.The impact of the factor such as shearing when but the sizing agent adding in slurry is subject to working condition as water quality, pH value, temperature and pumping, so the retention of sizing agent and effect all can be subject to impact to a certain extent.In addition, AKD and ASA molecule are nonionic organic matter, all without electropositivity, need first could form suction-operated to fiber by means of cationic emulsifier, thereby then AKD and ASA react and are bonded to fiber surface with cellulosic hydroxy again; AKD and ASA another problem in use is easily hydrolyzed exactly, and this just makes them not well to be applied in paper.
The occupation mode of another sizing agent is top sizing.Top sizing is exactly to become a certain amount of sizing agent of surface application of paper, and compared with the sizing agent adding in slurry, Cypres has many good qualities: it is not subject to the impact of copy paper water quality and water temperature, can obtain stable degree of sizing; The consumption that reduces sizing agent, reduces production costs, and reduces the obstacles such as machinery contamination, can make paper machine system more clean, reduces the COD of paper machine white water; The effect performance of Cypres does not need slaking etc.At present, use more Cypres can be divided into natural polymer subclass, as modified starch, and the Cypres of synthetic polymer class, as water-soluble polymer Cypres (styrene maleic anhydride copolymer, is called for short SMA and styrene acrylic copolymer, is called for short SAA).But these Cypres also have shortcoming separately, modified starch is owing to containing a lot of hydrophilic hydroxyls on strand, although WATER RESISTANCE is still poor so the paper surface strength of processing with such sizing agent increases.SMA, SAA are anionic polymer, can not in low pH environment, use, and often will be by some cationic substance competence exertion effect.In addition, this series products in use can produce a large amount of foams, thereby affects the stability of size press effect, has limited its application in paper industry.
Summary of the invention
Technical problem to be solved by this invention overcome the deficiencies in the prior art, a kind of new sizing agent is provided, this sizing agent not only can be for starching interior interpolation, can also be used for top sizing, no matter which kind of occupation mode can improve the WATER RESISTANCE of paper greatly, can increase the surface strength of paper simultaneously.
The present invention also provides the preparation method and application of this sizing agent simultaneously.
For overcoming the above problems, a kind of technical scheme that the present invention takes is as follows:
Sizing agent shown in a kind of formula (I),
The another technical scheme that the present invention takes is: a kind of preparation method of sizing agent, it comprises the steps:
(1) make hexadecylic acid and diethylenetriamine under catalyst exists and 90～180 DEG C of temperature at react and within 3～10 hours, obtain the fatty acid amide shown in formula (II),
CH
3(CH
2)
14CONHCH
2CH
2NHCH
2CH
2NHOC(CH
2)
14CH
3 (II)，
Wherein the mass ratio that feeds intake of hexadecylic acid and diethylenetriamine is 0.1～20:1;
(2) step (1) gained fatty acid amide is joined in reaction vessel, control temperature between 50 DEG C～95 DEG C and under stirring, add dimethyl carbonate and NaOH, the mass ratio that feeds intake of fatty acid amide and dimethyl carbonate is 0.05～25:1, the mass ratio of fatty acid amide and NaOH is 0.1～30:1, after adding, continue reaction 2～7 hours, obtain described sizing agent.
The related reaction of step (2) is expressed as follows with equation
In step (1), catalyst adds with the amount of catalysis, is generally hexadecylic acid and diethylenetriamine 0.01%～10% of the quality sum that feeds intake, and is preferably 0.1%～2%.Catalyst can be for being selected from sodium fluoride, sodium methoxide, and caustic alcohol, the combination of one or more in p-methyl benzenesulfonic acid, the quality that adds of catalyst is described aliphatic acid and diethylenetriamine 0.1%～2% of the quality sum that feeds intake.Preferred catalyst is p-methyl benzenesulfonic acid.
In step (1), preferred reaction temperature is 130～155 DEG C.The preferred reaction time is 4～8 hours.
In step (2), preferred reaction temperature is 65 DEG C～85 DEG C, and the preferred reaction time is 2～5 hours.
Preferably, the mass ratio that feeds intake of fatty acid amide and dimethyl carbonate is 1～10:1, more preferably 2～8:1, more preferably 3～6:1.Preferably, the mass ratio that feeds intake of fatty acid amide and NaOH is 1～20:1, and more preferably, the mass ratio that feeds intake of fatty acid amide and NaOH is 10～20:1.
The present invention also provides a kind of applying glue liquid, and it is mixed by the above-mentioned sizing agent of the present invention, emulsifying agent and water, and wherein, described emulsifying agent and water account for respectively 0.1wt%～40wt% and the 1wt%～95wt% of described applying glue liquid.
Further, emulsifying agent can be cationic, and macromolecular compound anion or non-ionic mainly contains higher fatty acids, higher aliphatic and their ester; Fatty alcohol-polyoxyethylene ether, the alkylphenol polyoxyethylene etc. of nonionic; Sodium alkyl sulfate, sodium alkyl sulfonate and the quaternary ammonium cation type of anionic.Concrete as cationic starch, polyamine, daiamid epoxy chloropropane etc.
The Surface sizing mechanism of application of sizing agents of the present invention on paper is as follows: because this sizing agent is the compound of cationic quaternary ammonium salt, itself belong to is from consolidating type sizing agent, so in the time that this material is applied on paper, electronegative fiber can be first makes sizing agent anchor at the surface of fiber with the fatty acid amide sizing agent generation Electrostatic Absorption with positive electricity, and the long carbon alkyl chain of this sizing agent can spread over the surface of paper and then play effect hydrophobic, water resistant.
Further, the sizing agent the present invention relates to can use separately in actual application, also can composite use together with other sizing agent, can plasm-glue-blending, and also can top sizing.For this reason, the invention still further relates to a kind of paper and/or cardboard glue applying method, take plasm-glue-blending mode or top sizing mode, the sizing agent that the method adopts at least comprises the above-mentioned sizing agent of the present invention.In addition the invention still further relates to by the paper after the method applying glue and/or cardboard.
Further, described Paper or cardboard can be cultural paper, industrial paper, and package paper, information paper using and special paper using, as: art paper, LWC, printing paper; Kraft liner, corrugating medium, coated white paperboard, chipboard; Wrapping paper, bag brown paper; Autotype paper, facsimile transmission paper, no carbon paper; Bank-note paper etc.And this Paper or cardboard is quantitative for being greater than 15g/m
2.In addition, the body paper of Paper or cardboard involved in the present invention is in the time manufacturing paper with pulp, and the raw material using can be pure wood pulp, straw pulp, and bamboo pulp, bagasse, agricultural crop straw, reclaims slurry, the mixture of any one or a few slurry wherein such as mineral filler.
According to a concrete aspect, the surface sizing method of described Paper or cardboard is as follows: by body paper by smooth being placed on sizing applicator of sizing applicator requirement, depress idler roller, again application roll is pressed in to top of form, put down fixed-wing, after the oxidized starch that the emulsion (applying glue liquid as above-mentioned in the present invention) that sizing agent of the present invention is made into and gelatinization are good or enzyme converted starch are composite, make it be evenly distributed in top of form, start button, completes the applying glue of paper.
According to a concrete aspect, the plasm-glue-blending method of described Paper or cardboard is as follows: according to the quantitative requirement of required paper of manufacturing paper with pulp, take a certain amount of certain density slurry preparing, the emulsion (applying glue liquid as above-mentioned in the present invention) that sizing agent of the present invention is made into joins in slurry, stir, handsheet.Certainly can also in the process of handsheet, add according to demand other chemicals, as dry strength agent, wet strength agent, retention agent etc.
Due to the employing of above technical scheme, the present invention compared with prior art tool has the following advantages:
Sizing agent of the present invention not only can, for starching interior interpolation, can also be used for top sizing, no matter which kind of occupation mode can improve the WATER RESISTANCE of paper greatly, can increase the surface strength of paper simultaneously.
Prepare gained sizing agent and overcome existing sizing agent and can only take a kind of deficiency of resin application methods by the preparation method of sizing agent of the present invention, no matter which kind of occupation mode can improve the WATER RESISTANCE of paper greatly, can increase the surface strength of paper, and this application of sizing agents scope is wide simultaneously.
Take the Paper or cardboard WATER RESISTANCE after glue applying method applying glue of the present invention good, surface strength is high.
Detailed description of the invention
Sizing agent of the present invention compared with existing synthetic class sizing agent (AKD, ASA), although three be all can with the reactive sizing agent of fiber-reactive, exist following significantly different:
1, AKD is nonionic organic matter, need to could form suction-operated to fiber by cationic emulsifier, secondly, the reactivity of AKD is more weak, react and generate β-carbonyl ester with fiber surface hydroxyl, this reaction needed regular hour and temperature, so used AKD applying glue to there will be applying glue hysteresis.
2, ASA is nonionic organic matter, also need to could form suction-operated to fiber by cationic emulsifier, secondly, ASA reactivity is strong, and poor stability, very easily with the substance reaction that contains active hydrogen, can produce very soon hydrolysis as contacted with water, so use ASA to need on-the-spot emulsification.
3, the sizing agent the present invention relates to belongs to the compound of cationic quaternary ammonium salt, compares with ASA with AKD, just can be adsorbed on fiber without the material by other, is a kind of without applying glue hysteresis, and the glue used in paper-making of stable performance.
4, there is the phenomenon of hydrolysis in sizing agent of the present invention, ASA and AKD, but sizing agent hydrolysis rate of the present invention is slower than AKD and ASA, hydrolysate has cationic, still can be adsorbed on fiber, so very little on the impact using, and the hydrolysis amplitude of AKD and ASA wants large many, can obviously have influence on use.
5, sizing agent of the present invention both can also can be for top sizing for starching interior interpolation, and AKD not only has the maturation period for top sizing, and because its essence is wax, can reduce the coefficient of friction of paper surface, thereby affect the runnability of paper on printing machine.
Below in conjunction with specific embodiment, the present invention is described in further details.Should be understood that these embodiment are for general principle of the present invention, principal character and advantage are described, and the present invention is not limited by the following examples.The implementation condition adopting in embodiment can be done further adjustment according to specific requirement, and not marked implementation condition is generally the condition in normal experiment.
Embodiment 1
1, the preparation of sizing agent
The first step: fatty acid amide synthetic
In the 1000ml four-hole boiling flask that agitator, thermometer and condenser pipe are housed, add a certain amount of reactant hexadecylic acid and diethylenetriamine, and a small amount of p-methyl benzenesulfonic acid, wherein the mass ratio of hexadecylic acid and diethylenetriamine is 4:1, the addition of p-methyl benzenesulfonic acid be above-mentioned reactant quality summation 0.8%, three is mixed, and it is 150 DEG C that heating makes the temperature of system, and the reaction time is 6 hours, make to react completely, the product of final gained is fatty acid amide.
Second step: fatty acid amide cation-modified
In the 1000ml four-hole boiling flask that agitator, thermometer, dropping funel and condenser pipe are housed, the fatty acid amide that adds the first step to make, adjust temperature, the temperature that makes system is 75 DEG C, drips a certain amount of dimethyl carbonate from dropping funel, the mass ratio that makes fatty acid amide and dimethyl carbonate is 3:1, in reaction system, add a certain amount of NaOH, make the mass ratio 15:1 of fatty acid amide and NaOH, drip rear continuation reaction 3 hours simultaneously, complete cation-modifiedly, obtain sizing agent.
2, the preparation of applying glue liquid
Take above-mentioned CATION fat acid amides, emulsifying agent daiamid epoxy chloropropane and water, mix three according to the ratio of mass ratio 9:9:82.
The preparation of the handsheet that 3, contains this sizing agent
The hardwood pulp that is 450ml freedom and freedom are that the softwood pulp of 550ml is that 8:2 mixes according to over dry mass ratio, be made into concentration and be 1.2% pulp solution, take a certain amount of above-mentioned applying glue liquid and join in slurry and stir, that take that a certain amount of this slurry handsheet makes handsheet is quantitatively 80g/m
2, the mass ratio of over dry applying glue liquid and oven dry stock is 0.2%.
In order to highlight the distinctive technique effect of sizing agent prepared by the present invention, the present invention carries out application experiment by homemade sizing agent with commercially available AKD together with ASA sizing agent, take respectively three kinds of sizing agents of identical oven-dry weight, mix with slurry, handsheet, then compare three's effect, applying glue stability and applying glue hysteresis quality, concrete experimental result is as follows:
1) the effect comparison of mill size and AKD and ASA, referring to table 1.
The effect comparison of three kinds of sizing agents of table 1
2) the stability comparison of mill size and AKD and ASA, referring to table 2.
The stability comparison of three kinds of sizing agents of table 2 under 60 DEG C of conditions of storage
3) the applying glue hysteresis quality comparison of mill size and AKD, referring to table 3.
The applying glue hysteresis quality comparison of two kinds of sizing agents of table 3
Embodiment 2
1, the preparation of sizing agent
The first step: fatty acid amide synthetic
In the 1000ml four-hole boiling flask that agitator, thermometer and condenser pipe are housed, add a certain amount of reactant hexadecylic acid and diethylenetriamine, and a small amount of sodium fluoride, wherein the mass ratio of hexadecylic acid and diethylenetriamine is 5:1, the addition of sodium fluoride be above-mentioned reactant quality summation 1.2%, three is mixed, and it is 160 DEG C that heating makes the temperature of system, and the reaction time is 5 hours, make to react completely, the product of final gained is fatty acid amide.
Second step: fatty acid amide cation-modified
In the 1000ml four-hole boiling flask that agitator, thermometer, dropping funel and condenser pipe are housed, the fatty acid amide that adds the first step to make, adjust temperature, the temperature that makes system is 70 DEG C, drips a certain amount of dimethyl carbonate from dropping funel, the mass ratio that makes fatty acid amide and dimethyl carbonate is 4:1, in reaction system, add a certain amount of NaOH, make the mass ratio 12:1 of fatty acid amide and NaOH, drip rear continuation reaction 3 hours simultaneously, complete cation-modifiedly, obtain sizing agent.
2, the configuration of surface size
The present embodiment adopts good oxidized starch and the homemade sizing agent of gelatinization to be combined together use, and oxidized starch is 97:3 with the over dry mass ratio of self-control Cypres, and the concentration of surface size is 8%, and the temperature of surface size is 60 DEG C.Wherein, mill size is actual is according to the mixed sizing agent of the ratio of mass ratio 11:8:81 with fatty alcohol-polyoxyethylene ether and water.
Note: the gelatinization technique of oxidized starch is as follows: add suitable quantity of water in reaction flask, oxidized starch is slowly added, uniform stirring, is heated to 90 DEG C, insulation 15min, being cooled to 60～70 DEG C can use.
The preparation of the paper that 3, contains this sizing agent
To be quantitatively 50g/m
2body paper by smooth being placed on sizing applicator of sizing applicator requirement, depress idler roller, then application roll be pressed in to top of form, put down fixed-wing, a certain amount of applying glue liquid is evenly distributed in to top of form, control resin added is 1.5g/m
2, start button, completes the applying glue experiment of paper.The paper that completes applying glue is placed on to laboratory with constant temperature and constant humidity equilibrium water conten and after 24 hours, carries out the detection of paper physical property.
In order to highlight the distinctive technique effect of sizing agent prepared by the present invention, the present invention carries out application experiment by homemade sizing agent with together with commercially available SMA sizing agent, be that both are combined together use with identical over dry mass ratio and oxidized starch, then both effects relatively, concrete experimental result is referring to table 4:
The effect comparison of two kinds of sizing agents of table 4
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (10)
1. the sizing agent shown in formula (I),
。
2. a preparation method for sizing agent, is characterized in that, comprises the steps:
(1) make hexadecylic acid and diethylenetriamine under catalyst exists and 90～180 DEG C of temperature at react and within 3～10 hours, obtain the fatty acid amide shown in formula (II),
CH
3(CH
2)
14CONHCH
2CH
2NHCH
2CH
2NHOC(CH
2)
14CH
3 (II)，
Wherein the mass ratio that feeds intake of hexadecylic acid and diethylenetriamine is 0.1～20:1;
(2) step (1) gained fatty acid amide is joined in reaction vessel, control temperature between 50 DEG C～95 DEG C and under stirring, add dimethyl carbonate and NaOH, the mass ratio that feeds intake of fatty acid amide and dimethyl carbonate is 0.05～25:1, the mass ratio of fatty acid amide and NaOH is 0.1～30:1, after adding, continue reaction 2～7 hours, obtain described sizing agent.
3. the preparation method of sizing agent according to claim 2, it is characterized in that: in step (1), described catalyst is for being selected from sodium fluoride, sodium methoxide, caustic alcohol, the combination of one or more in p-methyl benzenesulfonic acid, the quality that adds of described catalyst is described aliphatic acid and diethylenetriamine 0.1%～2% of the quality sum that feeds intake.
4. according to the preparation method of the sizing agent described in claim 2 or 3, it is characterized in that: in step (1), reaction is carried out at 130～155 DEG C of temperature, the reaction time is 4～8 hours.
5. the preparation method of sizing agent according to claim 2, is characterized in that: in step (2), reaction is carried out at 65 DEG C～85 DEG C of temperature, the reaction time is 2～5 hours.
6. paper and/or a cardboard glue applying method, takes plasm-glue-blending mode or top sizing mode, it is characterized in that: the sizing agent that described method adopts at least comprises sizing agent claimed in claim 1.
7. take paper and/or the cardboard after method applying glue described in claim 6 for one kind.
8. an applying glue liquid, is characterized in that: it is mixed by sizing agent claimed in claim 1, emulsifying agent and water, and described emulsifying agent and water account for respectively 0.1wt%～40wt% and the 1wt%～95wt% of described applying glue liquid.
9. applying glue liquid according to claim 8, is characterized in that, described emulsifying agent is selected from: higher fatty acids, higher aliphatic and their ester; The fatty alcohol-polyoxyethylene ether of nonionic, alkylphenol polyoxyethylene; Sodium alkyl sulfate, sodium alkyl sulfonate and the quaternary ammonium cation type emulsifying agent of anionic.
10. the application of the applying glue liquid described in claim 8 or 9 in paper and/or cardboard applying glue.
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| CN106676961A (en) * | 2016-12-09 | 2017-05-17 | 苏州艾博迈尔新材料有限公司 | Modified hogskin collagen sizing agent and preparation method thereof |
| CN108221474A (en) * | 2018-01-11 | 2018-06-29 | 石家庄德旺科技有限公司 | A kind of preparation method of new paper making glue |
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| CN1443899A (en) * | 2002-03-12 | 2003-09-24 | 牛华 | Preparation method of rosen polyester sizing agent |
| CN101435173A (en) * | 2008-12-22 | 2009-05-20 | 陕西科技大学 | Paper making neutral sizing agent and preparing method thereof |
| CN101509213A (en) * | 2009-03-27 | 2009-08-19 | 上海应用技术学院 | Bisamide quaternary ammonium salt sheet softening agent, preparation and uses thereof |
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| JP2003089995A (en) * | 2001-07-10 | 2003-03-28 | Arakawa Chem Ind Co Ltd | Sizing agent for making paper |
| CN1443899A (en) * | 2002-03-12 | 2003-09-24 | 牛华 | Preparation method of rosen polyester sizing agent |
| CN101435173A (en) * | 2008-12-22 | 2009-05-20 | 陕西科技大学 | Paper making neutral sizing agent and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106676961A (en) * | 2016-12-09 | 2017-05-17 | 苏州艾博迈尔新材料有限公司 | Modified hogskin collagen sizing agent and preparation method thereof |
| CN108221474A (en) * | 2018-01-11 | 2018-06-29 | 石家庄德旺科技有限公司 | A kind of preparation method of new paper making glue |
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