CN1109125A - Manufacture of neutral adhesive-applied fiber of alkyl ketene dipolymer - Google Patents

Manufacture of neutral adhesive-applied fiber of alkyl ketene dipolymer Download PDF

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CN1109125A
CN1109125A CN 94108681 CN94108681A CN1109125A CN 1109125 A CN1109125 A CN 1109125A CN 94108681 CN94108681 CN 94108681 CN 94108681 A CN94108681 A CN 94108681A CN 1109125 A CN1109125 A CN 1109125A
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paper
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alkyl ketene
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CN1045216C (en
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朱国华
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Abstract

The process for preparing adhesive-applying neutral fibre of alkyl ketene dipolymer (AKD) includes such technological steps as fusing solid AKD, adding surfactant and solvent for emulsifying, modifying paper fibre with emulsified liquid, and solvent separation. It may be stored at 50 deg.C for a long time if it is not in touch with water. The paper pulp beated after be added the fibre may be stored at ordinary temp. for 24 hrs.

Description

Manufacture of neutral adhesive-applied fiber of alkyl ketene dipolymer
The present invention relates to alkyl ketene dimer (AKD) neutral sizing fiber preparation method.
Neutral sizing is the main developing direction of world today's paper-making industry, and AKD is the neutral sizing agent of consumption maximum in the neutral papermaking.
The AKD neutral sizing agent is a kind of reactive sizing agent, by U.S. Hercules company, at first released in 1984, by for improve and perfect disconnectedly, the AKD neutral sizing agent has embodied fully: can use cheap pearl filler and cheap broken in manufacturing paper with pulp, also improve simultaneously the intensity of paper and the ability of resisting lactic acid, and copy the sweat disadvantage that paper paper feeding and paper machine bring under the acid condition having reduced greatly, whiteness, pliability, opacity at paper, paper under solar radiation, the obvious superiority of aspects such as storage period.
The AKD neutral sizing agent that occurs in the world all is a water-based emulsion at present, and AKD content is 8~15%, and the applying glue consumption is heavy at 0.2~0.4%(AKD weight/paper oven dry stock), the paper of applying glue liquid, suddenly (Cobb) value is at Cobb 3016~40.AKD neutral sizing water-based emulsion, more convenient in the use, add the groove that to control flow at the flow box place, adding one at flow box stirs at once, cobb value is also quite desirable, but the shortcoming of AKD neutral sizing water-based emulsion maximum is: very easily hydrolysis behind the lactone ring chance water in the AKD structure generates ketone, and emits CO after the hydrolysis 2Gas, the AKD after the hydrolysis does not have sizing efficiency, and can cause deposition to cause obstacle, as roll banding, sticking pressure roller, foam increase, the white water recycle difficulty.According to the data report, AKD stirred 60 minutes in 30 ℃ water, and the 30% generation hydrolysis of just having an appointment was stirred 10 minutes in 70 ℃ water, and hydrolysis was put four hours at 37.7 ℃ up to 60%, and also the loss of energy 5%, and structure and the hydrolyzing type of AKD are shown below:
A. neutral sizing agent AKD general formula:
Figure 94108681X_IMG1
In the formula: R represents to have the alkyl of 4~16 carbon atoms.
B.AKD hydrolysis formula:
Figure 94108681X_IMG2
AKD neutral sizing water-based emulsion, at normal temperatures, about 3 months of maintenance phase, bring the summer of a lot of difficulties, particularly torrid areas and southern china for transportation and storage almost is the transportation and the storage of this water-based emulsion of incompatibility for this reason.
The purpose of this invention is to provide a kind of the 50 ℃ of alkyl ketene dimer neutral sizing fiber preparation method that can preserve for a long time down.
The present invention takes following measures in order to achieve the above object, and it comprises:
A) pulverizing of pulpboard
Paper fiber parent adopts the pulp board of needlebush, leaf wood, awns bar, alfa, wooden class to become the loose byssaceous paper fiber that does not have pulpboard point basically in crusher for crushing;
B) emulsification
Get AKD3.2~70 part, add paraffin wax and add the emulsification still for 1~28 part, be heated to 60~85 ℃, stir after the fusion, mixing speed is controlled at 1400~3000 rev/mins, drip surfactant after 10~20 minutes, added in 7~20 minutes, and be cooled to 50~65 ℃, solubilizer 800~1500ml, keep 40~50 ℃ of temperature, stirred 30~60 minutes;
C) fibre modification
Get 100 parts of paper fibers after the pulverizing, add the sex change still, be heated to 70~90 ℃, under vacuum, stirred 30~50 minutes, and be cooled to 45 ℃ after eliminating water, be depressurized to normal pressure, add above-mentioned emulsion, remain on 40~50 ℃ and stirred 30~50 minutes down, heat up gradually to remove under vacuum and desolvate, release goes out product.
The present invention utilizes AKD facile hydrolysis in water, and under the little condition of butt or humidity, has goodish stability (never degenerating in 1~2 year), make parent with the paper fiber, surfactant and solvent are mediated, adopt AKD in short time and water or the paper fibre modification technology that do not contact with water, make profile such as byssaceous AKD neutral sizing fiber, this fiber can be preserved (not meeting water) for a long time under 50 ℃.Transportation and store very conveniently, it is also convenient than water-based emulsion to use, and need not add equipment, only needs and pulp board is pulled an oar together, and sizing efficiency is also good than water-based emulsion, and the applying glue consumption is 0.15~0.4%, and the cobb value scope is at Cobb 3010~32, when reaching the rosin sizing efficiency, near the rosin of traditional cheapness, its another advantage is the paper pulp that adds after AKD neutral sizing fiber is pulled an oar to ton paper applying glue cost, at room temperature places 24 hours, and cobb value is constant substantially.The preparation of this fiber, AKD content 30.5%, about 1.3 ten thousand yuan of expense of raw materials per ton, if on selling price 2.5 ten thousand yuan/ton, about 153 yuan of 0.2% ton of paper applying glue of applying glue consumption expense, the rosin applying glue expense (130 yuan) of approaching at present traditional cheapness.
Surfactant among the above-mentioned preparation method can adopt alkyltrimethyl ammonium chloride, domestic trade mark X31, x=12~16; Alkylphenol polyoxyethylene, domestic trade mark OP-n 1, n 1=6~12; The oleic acid ethylene oxide adduct, O-n 2, n 2Be oxirane adduct number, n 2Be oxirane adduct number n 2=4~9; Solvent is a kind of media, does not influence product quality after eliminating in product, can adopt mixture, benzene, the toluene of ethanol, benzinum, ethanol and benzinum.
Embodiment 1
With the reed pulpboard, dry method is ground into loose byssaceous paper fiber in pulverizer, stand-by.Get AKD3.2g, paraffin wax 10g adds the emulsification still and is heated to 65~70 ℃, opens stirring after the fusion, about 2800 rev/mins of mixing speed; Get 1231 cationic surfactant 1.3g after 20 minutes; OP-10,0.7g; 0-7,1.6g dripped 10 minutes after evenly mixing, and were cooled to 50 ℃; Get benzinum 15ml, ethanol (95%) 800ml behind the mixing, slowly adds in the emulsification still; Remaining on 40 ℃ stirred 30 minutes down.Get the paper fiber 100g after the pulverizing, add in the sex change still, be heated to 85 ℃, under-0.08MPa pressure, stirred 40 minutes, be cooled to 45 ℃, be depressurized to normal pressure, add above-mentioned emulsion, remain on 45 ℃ and stirred 30 minutes down, under-0.08MPa, be warming up to 70 ℃ gradually and remove and desolvate, take out product after the release, promptly make AKD content and be 3.0% neutral sizing fiber.
Embodiment 2
With the needlebush pulpboard, dry method is ground into loose byssaceous paper fiber in pulverizer, stand-by.Get AKD70g, paraffin wax 3g adds the emulsification still, is heated to 65~70 ℃, opens stirring after the fusion, and about 2800 rev/mins of mixing speed is got 1231 cationic surfactant 10.5g after 20 minutes; OP-10,7g; 0-7,14g add 10 minutes after evenly mixing, and are cooled to 50 ℃, get benzinum 26.7ml, and ethanol (95%) 800ml slowly adds in the still behind the mixing, remain on 40 ℃ and stir 30 minutes down.Get the fiber 100g after the pulverizing, add in the sex change still, be heated to 85 ℃, under-0.08MPa pressure, stirred 40 minutes, be cooled to 45 ℃, be depressurized to normal pressure, add above-mentioned emulsion, remaining on 45 ℃ stirred 30 minutes down, under-0.08MPa, be warming up to 70 ℃ gradually, remove and desolvate, after the release, take out product, promptly make AKD content and be 30.5% neutral sizing fiber.

Claims (3)

1, a kind of alkyl ketene dimer neutral sizing fiber preparation method is characterized in that it comprises:
A) pulverizing of pulpboard
Paper fiber parent adopts the pulp board of needlebush, leaf wood, awns bar, alfa, wooden class to become the loose byssaceous paper fiber that does not have pulpboard point basically in crusher for crushing;
B) emulsification
Get AKD3.2~70 part, add paraffin wax and add the emulsification still for 1~28 part, be heated to 60~85 ℃, stir after the fusion, mixing speed is controlled at 1400~3000 rev/mins, drip surfactant after 10~20 minutes, added in 7~20 minutes, and be cooled to 50~65 ℃, solubilizer 800~1500ml, keep 40~50 ℃ of temperature, stirred 30~60 minutes;
C) fibre modification
Get 100 parts of paper fibers after the pulverizing, add the sex change still, be heated to 70~90 ℃, under vacuum, stirred 30~50 minutes, and be cooled to 45 ℃ after eliminating water, be depressurized to normal pressure, add above-mentioned emulsion, remain on 40~50 ℃ and stirred 30~50 minutes down, heat up gradually to remove under vacuum and desolvate, release goes out product.
2, a kind of alkyl ketene dimer neutral sizing fiber preparation method according to claim 1 is characterized in that said surfactant adopts alkyltrimethyl ammonium chloride, domestic trade mark X31, x=12~16; Alkylphenol polyoxyethylene, domestic trade mark OP-n 1, n 1=6~12; The oleic acid ethylene oxide adduct, O-n 2, n 2Be oxirane adduct number, n 2Be oxirane adduct number n 2=4~9.
3, a kind of alkyl ketene dimer neutral sizing fiber preparation method according to claim 1 and 2 is characterized in that said solvent adopts the mixture of ethanol, benzinum, ethanol and benzinum, benzene, toluene.
CN94108681A 1994-09-10 1994-09-10 Manufacture of neutral adhesive-applied fiber of alkyl ketene dipolymer Expired - Fee Related CN1045216C (en)

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CN94108681A CN1045216C (en) 1994-09-10 1994-09-10 Manufacture of neutral adhesive-applied fiber of alkyl ketene dipolymer

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CN1045216C CN1045216C (en) 1999-09-22

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100415991C (en) * 2002-12-17 2008-09-03 凯米罗总公司 Alkenylsuccinic anhydride compositions and method for using the same
CN102230297A (en) * 2011-06-13 2011-11-02 东北林业大学 Plant paper pulp fiber modifying agent and modifying method using same, and filter paper and preparation method thereof
CN103930618A (en) * 2011-11-14 2014-07-16 巴斯夫欧洲公司 Akd composition and manufacture of paper and paperboard
CN107727782A (en) * 2017-10-12 2018-02-23 华南理工大学 A kind of method of ionic liquid auxiliary headspace gas Chromatographic Determination AKD emulsion effective contents
CN108330738A (en) * 2018-02-12 2018-07-27 广东轻工职业技术学院 Complex fiber material and the preparation method and application thereof for top sizing

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69231379T2 (en) * 1991-03-01 2001-03-01 E.I. Du Pont De Nemours And Co., Wilmington SURFACE TREATED ARAMID FIBERS AND METHOD FOR THE PRODUCTION THEREOF
FI94535C (en) * 1992-12-04 1997-04-08 Raisio Chem Oy Process for preparing a hydrophobic dispersion

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100415991C (en) * 2002-12-17 2008-09-03 凯米罗总公司 Alkenylsuccinic anhydride compositions and method for using the same
CN102230297A (en) * 2011-06-13 2011-11-02 东北林业大学 Plant paper pulp fiber modifying agent and modifying method using same, and filter paper and preparation method thereof
CN102230297B (en) * 2011-06-13 2013-01-09 东北林业大学 Plant paper pulp fiber modifying method, and filter paper and preparation method thereof
CN103930618A (en) * 2011-11-14 2014-07-16 巴斯夫欧洲公司 Akd composition and manufacture of paper and paperboard
US9359724B2 (en) 2011-11-14 2016-06-07 Kemira Oyj AKD composition and manufacture of paper and paperboard
CN103930618B (en) * 2011-11-14 2016-06-08 凯米拉公司 The production of AKD composition and paper and paperboard
CN107727782A (en) * 2017-10-12 2018-02-23 华南理工大学 A kind of method of ionic liquid auxiliary headspace gas Chromatographic Determination AKD emulsion effective contents
CN107727782B (en) * 2017-10-12 2020-04-28 华南理工大学 Method for determining effective content of AKD emulsion by ionic liquid-assisted headspace gas chromatography
CN108330738A (en) * 2018-02-12 2018-07-27 广东轻工职业技术学院 Complex fiber material and the preparation method and application thereof for top sizing

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