CN102337707A - Preparation method of modified AKD (Alkyl Ketene Dimer) neutral sizing agent - Google Patents
Preparation method of modified AKD (Alkyl Ketene Dimer) neutral sizing agent Download PDFInfo
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- CN102337707A CN102337707A CN2011102924161A CN201110292416A CN102337707A CN 102337707 A CN102337707 A CN 102337707A CN 2011102924161 A CN2011102924161 A CN 2011102924161A CN 201110292416 A CN201110292416 A CN 201110292416A CN 102337707 A CN102337707 A CN 102337707A
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Abstract
The invention relates to a modified AKD (Alkyl Ketene Dimer) neutral sizing agent which is a milk white liquid in appearance. The modified AKD neutral sizing agent comprises the following main materials: AKD, starch, paraffin, high molecular dispersant and other assistant materials. The modified AKD neutral sizing agent is mainly used for sizing paper pulp and improving the water resistance and impermeability of paper in the paper-making production process, and the consumption for every ton of paper is 10-20kg. Compared with like products, the quickly-cured modified AKD neutral sizing agent has the following advantages: (1) effective ingredient particles of the product are finer and more uniform and can be cured more tightly, the product has a longer quality guarantee period, and convenience is provided for transportation and storage; (2) the product is applicable to neutral paper pulp and can no longer result in the production of acidic paper-making sewage, thereby being beneficial to environmental protection; (3) the use effect of the product can act quickly, and the curing time is extremely short, thereby facilitating the effect monitoring and quality control in use, improving the production efficiency and enhancing the yield of paper; and (4) the consumption of the product is lower than that of other like products, thereby reducing the cost of production materials and improving the economic benefits of customers.
Description
Technical field
The invention belongs to a kind of preparation technology of fine chemical material, explanation more specifically relates to a kind of preparation method of paper grade (stock) modification AKD neutral sizing agent.
Background technology
Existing like product mainly contains products such as common AKD emulsion, dispersion rosin size, ASA emulsion on the market, and this several prods all has weak point:
Example one: common AKD emulsion: (1) maturation period is long, and effect manifests slowly; (2) particulate in the product is gathered into bulky grain easily; (3) in the use, paper is prone to skid.
Example two: dispersion rosin size: (1) is not suitable for the use of neutral paper pulp; (2) be prone to layering, the shelf-life is short; (3) need to cooperate other aluminium salt raw materials to use and just produce effect, client's production cost is high.
Example three: ASA emulsion: (1) shelf-life is short, stores inconvenient; (2) use preceding on-the-spot emulsification, the troublesome poeration of needing; Difficult control when (3) using, effect is unstable.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of modification AKD neutral sizing agent; With alkyl ketene dimer, paraffin, aluminum sulfate is main raw material; Add promoter materials such as special-purpose self-control macromolecule dispersing agent, special-purpose self-control starch sizing, carry out high speed shear emulsification, high-pressure homogeneous reaction; Behind the preparation technologies such as quick cooling, make finished product.
To achieve these goals, the present invention adopts following technical scheme:
Modification AKD neutral sizing agent, its preparation method are with dispersant and starch sizing and a certain amount of dilution water, are heated to 80-90 ℃ after the mixing; After add alkyl ketene dimer, paraffin again and combine the blend glue stuff that generates, between 60-80 ℃, carried out at a high speed (1500r/min) emulsion reaction 15 minutes, feed the high pressure homogenizer of 40MPa again; The decompression homogeneous, sizing material is through plate type heat exchanger, after cooling off fast behind the homogeneous; Add a certain amount of dilution water and aluminum sulfate solution, be prepared as finished product.
The part by weight of each component of the present invention is: alkyl ketene dimer: paraffin: dispersant: starch sizing: aluminum sulfate solution: dilution water=90:10:100:100:200:500.
Alkyl ketene dimer of the present invention is that (in the synthesis material, the aliphatic acid of 18 carbochain numbers contains 40% to 1840 types.) alkyl ketene dimer.
Paraffin of the present invention is No. 58 paraffin wax fully refineds.
Dispersant of the present invention is polymerized with various chemical monomers and other chemical material.Be that oxidized tapioca is dissolved into sizing material, add NaOH (99%) and carry out substitution reaction, and dropping 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (69%) carry out graft reaction.Add glacial acetic acid again, acrylamide solution (40%), N hydroxymethyl acrylamide solution carries out polymerization, controls molecular weight with tert-dodecyl mercaptan, makes initator with ammonium persulfate.Add di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate again, to improve dispersive property.
Starch sizing of the present invention is to be that main raw material is polymerized with the cation cassava starch.Before this cation cassava starch was dissolved into sizing material, was heated to 90 ℃ of-95 ℃ of following gelatinizations, carried out " liquefaction " effect with α type amylase; а in the hydrolyzed starch molecule-1.4 glucoside bond generates short chain dextrin and a spot of low-molecular-weight carbohydrate, adds acrylamide solution (40%) again; Add dimethyl diallyl ammonium chloride and carry out polymerization, make initator, again with glacial acetic acid adjustment pH value with ammonium persulfate; Add shitosan polymerization again, to improve retention performance.
Aluminum sulfate solution of the present invention is the solution of no swage aluminum sulfate (alundum (Al content >=16.5%) in water.The part by weight of said each component is: no swage aluminum sulfate: water=100:150.
Water of the present invention is deionized water.
With existing compared with techniques; The present invention successfully introduces paraffin in the production of AKD neutral sizing agent; Improved the WATER RESISTANCE of AKD neutral sizing agent class, the present invention successfully synthesizes a kind of dispersant, and this is a kind of high molecular dispersant; Performances such as emulsibility, stability and permeability are preferably arranged, make the associating material of alkyl ketene dimer and paraffin be easier to dissolving, disperse.The present invention successfully synthesizes starch sizing, and this is a kind of high molecular retention agents, has improved the stability and the applying glue efficient of product.With associating material, synthetic dispersing agent, the starch sizing of alkyl ketene dimer and paraffin, through high speed shear emulsification and high-pressure homogeneous reaction, Sheng Shiyi colloidal sol body adds aluminum sulfate solution and dilution water again, the modification AKD neutral sizing agent of processing.This constant product quality, the product effect manifests soon, and consumption is little, and service efficiency is high, and use cost is low.
The specific embodiment
1, preparation dispersant
In enamel reaction still, feed intake:
1.1, composition of raw materials: by producing 1000.0 kilograms
1.1.1, oxidized tapioca: 108.0 kilograms; The MS-01 type starch that oxidized tapioca is produced by the bright positive biochemical industry in Guangxi Co., Ltd.
1.1.2, NaOH (99%): 7.5 kilograms;
1.1.3,69%3-chloro-2-hydroxypropyl-trimethyl ammonium chloride: 38.0 kilograms
1.1.4, tert-dodecyl mercaptan: 2.0 kilograms;
1.1.5, N hydroxymethyl acrylamide solution: 2.5 kilograms of N hydroxymethyl acrylamides add 40.0 kilograms of dissolvings of water, mix;
1.1.6,40% acrylamide solution: 178.0 kilograms;
1.1.7, the TX-10 emulsifier solution: 5 kilograms of TX-10 emulsifying agents add 25 kilograms of dissolvings of water, mix;
1.1.8, glacial acetic acid: 14.0 kilograms;
1.1.9, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate: 13.0 kilograms;
1.1.10, ammonium persulfate solution: 3.0 kilograms of ammonium persulfates add 80 kilograms of dissolvings of water, mix.
1.1.11, water: 484.0 kilograms
1.2, in the production technology of 1000 liters of reaction kettle for reaction
1.2.1,238.0 kg of water are added agitated reactor, stir and add oxidized tapioca down, when being heated to 40 ℃, isothermal reaction 30 minutes;
1.2.2, add NaOH (99%), when being heated to 60-65 ℃, isothermal reaction 30 minutes begins to drip 69%3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, after be heated to 70 ℃ of-75 ℃ of following isothermal reactions 3 hours;
1.2.3, add 86.0 kg of water, add glacial acetic acid, add 40% acrylamide solution, add tert-dodecyl mercaptan again, logical nitrogen 30 minutes;
1.2.4, begin to drip emulsifying agent (TX-10) solution again, drip N hydroxymethyl acrylamide solution simultaneously, dripped in 30 minutes; Drip ammonium persulfate solution simultaneously; Dripped 5/6ths of solution in 40 minutes, and stayed surplus sixth, material was 85 ℃ of-88 ℃ of following insulation reaction 1 hour;
1.2.5, dripped with 10 minutes and stay surplus ammonium persulfate solution again, material was 78 ℃ of-82 ℃ of following insulation reaction 2 hours; Add 160.0 kilograms in water, add dispersant N, be warming up to 90 ℃, be incubated 30 minutes, be cooled to 50 ℃ and get final product blowing, be these article dispersant special.
1000 kilograms in water, 100 kilograms of CMSs, thrown material after, stirred 30 minutes, after be warming up to more than 90 ℃, timing insulated and stirred 2 hours is cooled to 60 ℃ of blowings, mistake 80 mesh sieves are crossed and are filtered CMS gelatinization sizing material.
2, preparation starch sizing
In enamel reaction still, feed intake:
2.1, composition of raw materials: by producing 1000.0 kilograms
2.1.1, cation cassava starch: 125.0 kilograms; The CS-08 type starch that cation cassava starch is produced by the bright positive biochemical industry in Guangxi Co., Ltd.
2.1.2, α type amylase: 0.15 kilogram;
2.1.3,40% acrylamide solution: 35.0 kilograms;
2.1.4, dimethyl diallyl ammonium chloride: 50.0 kilograms;
2.1.5, shitosan: 1.1 kilograms;
2.1.6, glacial acetic acid: 14.0 kilograms;
2.1.7, ammonium persulfate solution: 2.75 kilograms add 45.0 kilograms of dissolvings of water, mix.
2.1.8, water: 727.0 kilograms.
2.2, in the production technology of 1000 liters of reaction kettle for reaction
2.2.1, add 400.0 kg of water, add cation cassava starch, add α type amylase after, be heated to 90 ℃ of-95 ℃ of following isothermal reactions 1 hour;
2.2.2, add 80.0 kg of water, 40% adds acrylamide solution, stirs to add dimethyl diallyl ammonium chloride down, logical nitrogen dripped ammonium persulfate solution 2 hours, when being heated to 80-82 ℃, isothermal reaction 3 hours;
2.2.3, stop logical nitrogen, add 247.0 kg of water, add glacial acetic acid, add shitosan, be warming up to 90 ℃, be incubated 2 hours, be cooled to 50 ℃ and get final product blowing, be the starch specialized sizing material of these article.
3, preparation aluminum sulfate solution
In enamel reaction still, feed intake: 400.0 kilograms of no swage aluminum sulfate are added in 600.0 kg of water, stir more than 1 hour, till the dissolving of the solids overwhelming majority, filter after 100 eye mesh screens.
4, preparation finished product
4.1, in stainless steel cauldron, feed intake: 90.0 kilograms of alkyl ketene dimers and 10.0 kilograms of paraffin, be melted up to 65-70 ℃, stir;
4.2, in the emulsify at a high speed jar of 1500r/min, feed intake: 100.0 kilograms the self-control dispersant specials, 100.0 kilograms the self-control starch specialized sizing materials, 300.0 kg of water after the stirring, are heated to 85-90 ℃;
4.3, with the alkyl ketene dimer and the paraffin compound that melt, add in the material of emulsify at a high speed jar of 1500r/min, sheared 15 minutes through high speed dispersion, blowing filters through 80 eye mesh screens, obtains the dispersion and emulsion sizing material;
4.4, the dispersion and emulsion sizing material fed the high pressure homogenizer of 40MPa; The decompression homogeneous, behind the homogeneous sizing material through plate type heat exchanger, be quickly cooled to 25-30 ℃ after; Add 200.0 kilograms of dilution waters and 200.0 kilograms of aluminum sulfate solutions; After stirring, filter, promptly be prepared as finished product through 100 eye mesh screens.
Claims (8)
1. modification AKD neutral sizing agent is characterized in that, its preparation method is with dispersant and starch sizing and a certain amount of dilution water; Be heated to 80-90 ℃ after the mixing, after add alkyl ketene dimer, paraffin again and combine the blend glue stuff that generates, between 60-80 ℃, carry out the emulsify at a high speed reaction 15 minutes of 1500r/minr; Feed the high pressure homogenizer of 40MPa again; The decompression homogeneous, sizing material is through plate type heat exchanger, after cooling off fast behind the homogeneous; Add a certain amount of dilution water and aluminum sulfate solution, be prepared as finished product.
2. modification AKD neutral sizing agent according to claim 1, it is characterized in that: the part by weight of described each component is: alkyl ketene dimer: paraffin: dispersant: starch sizing: aluminum sulfate solution: dilution water=90:10:100:100:200:500.
3. modification AKD neutral sizing agent according to claim 1 is characterized in that: described alkyl ketene dimer is 1840 type alkyl ketene dimers, and in the synthesis material, the aliphatic acid of 18 carbochain numbers contains 40%.
4. modification AKD neutral sizing agent according to claim 1 is characterized in that: described paraffin is No. 58 paraffin wax fully refineds.
5. modification AKD neutral sizing agent according to claim 1; It is characterized in that: described dispersant is polymerized with various chemical monomers and other chemical material; Be that oxidized tapioca is dissolved into sizing material; Add NaOH (99%) and carry out substitution reaction, and dropping 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (69%) carries out graft reaction; Add glacial acetic acid again, acrylamide solution (40%), N hydroxymethyl acrylamide solution carries out polymerization, controls molecular weight with tert-dodecyl mercaptan, makes initator with ammonium persulfate, adds di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate again, to improve dispersive property.
6. modification AKD neutral sizing agent according to claim 1 is characterized in that: described starch sizing is to be that main raw material is polymerized with the cation cassava starch, before this cation cassava starch is dissolved into sizing material; Be heated to 90 ℃ of-95 ℃ of following gelatinizations, carry out " liquefaction " effect, а in the hydrolyzed starch molecule-1.4 glucoside bond with α type amylase; Generate short chain dextrin and a spot of low-molecular-weight carbohydrate, add acrylamide solution (40%) again, add dimethyl diallyl ammonium chloride and carry out polymerization; Make initator with ammonium persulfate; With glacial acetic acid adjustment pH value, add shitosan polymerization again, again to improve retention performance.
7. modification AKD neutral sizing agent according to claim 1; It is characterized in that: aluminum sulfate solution is the solution of no swage aluminum sulfate (alundum (Al content >=16.5%) in water, and the part by weight of its each component is: no swage aluminum sulfate: water=100:150.
8. modification AKD neutral sizing agent according to claim 1 is characterized in that: described water is deionized water.
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| CN102627733A (en) * | 2012-05-04 | 2012-08-08 | 陕西科技大学 | Preparation method of high-activity half-crosslinking amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent |
| CN102635028A (en) * | 2012-05-04 | 2012-08-15 | 陕西科技大学 | Preparation method for cation sweet potato starch microcrystalline wax/alkyl ketene dimer (AKD) neutral/basic sizing agent |
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| CN103524462B (en) * | 2013-10-16 | 2015-05-06 | 上海东升新材料有限公司 | Modified alkyl ketene dimer and preparation method thereof |
| CN104452450A (en) * | 2014-11-06 | 2015-03-25 | 江苏理文造纸有限公司 | High-gluing rapid curing type AKD (alkyl ketene dimer) emulsion and papermaking process using same |
| CN104452450B (en) * | 2014-11-06 | 2017-04-05 | 江苏理文造纸有限公司 | High applying glue rapid maturing type AKD emulsions and the paper technology using the emulsion |
| CN106351067A (en) * | 2016-09-20 | 2017-01-25 | 广东志造生物科技有限公司 | Paper surface sizing agent and sizing method thereof |
| CN106676974A (en) * | 2017-01-23 | 2017-05-17 | 北京中科奥倍超声波技术研究院 | Method for preparing environment-friendly damp-proof plate |
| CN107558297A (en) * | 2017-09-08 | 2018-01-09 | 湖北金庄科技再生资源有限公司 | A kind of waterproof and dampproof enhanced sizing agent and preparation method thereof |
| CN108330737A (en) * | 2017-12-30 | 2018-07-27 | 重庆理文造纸有限公司 | A kind of Cypres and preparation method thereof improving paper web water-resistance |
| CN108330737B (en) * | 2017-12-30 | 2021-04-20 | 重庆理文造纸有限公司 | Surface sizing agent for improving water resistance of paper web and preparation method thereof |
| CN108455805A (en) * | 2018-04-03 | 2018-08-28 | 晋州市大成变性淀粉有限公司 | A kind of preparation method of sludge recovery agent |
| CN111395036A (en) * | 2020-03-23 | 2020-07-10 | 抚州市鹤达实业有限公司 | Solid surface sizing agent for paper making |
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