CN102337707B - 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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- CN102337707B CN102337707B CN 201110292416 CN201110292416A CN102337707B CN 102337707 B CN102337707 B CN 102337707B CN 201110292416 CN201110292416 CN 201110292416 CN 201110292416 A CN201110292416 A CN 201110292416A CN 102337707 B CN102337707 B CN 102337707B
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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, more specific description relates to a kind of preparation method of paper grade (stock) modification AKD neutral sizing agent.
Background technology
On market, existing like product mainly contains the products such as common AKD emulsion, dispersion rosin size, ASA emulsion, and this several prods has weak point:
Example one: common AKD emulsion: (1) maturation period is long, and effect manifests slowly; (2) particulate in product easily is gathered into bulky grain; (3) in use procedure, paper easily skids.
Example two: dispersion rosin size: (1) is not suitable for the use of neutral paper pulp; (2) easily layering, the shelf-life is short; (3) need to coordinate 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) need on-the-spot emulsification, troublesome poeration before the use; (3) difficult control while applying, 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, take alkyl ketene dimer, paraffin, aluminum sulfate is main raw material, add the 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, fast, after the preparation technology such as cooling, make finished product.
To achieve these goals, the present invention adopts following technical scheme:
Modification AKD neutral sizing agent, its preparation method is by dispersant and starch sizing and a certain amount of dilution water, be heated to 80-90 ℃ after mixing, after add again alkyl ketene dimer, paraffin in conjunction with the blend glue stuff generated, carry out high speed (1500r/min) emulsion reaction 15 minutes between 60-80 ℃, pass into again the high pressure homogenizer of 40MPa, the decompression homogeneous, after homogeneous, sizing material passes through plate type heat exchanger, carry out fast cooling after, 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 synthesis material, the aliphatic acid of 18 carbochain numbers is containing 40% for 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 to sizing material, add NaOH (99%) to carry out substitution reaction, and the dropping chloro-2-hydroxypropyl-trimethyl ammonium chloride of 3-(69%) carries out graft reaction.Add again glacial acetic acid, acrylamide solution (40%), N hydroxymethyl acrylamide solution carries out polymerization, with tert-dodecyl mercaptan, controls molecular weight, with ammonium persulfate, makes initator.Add again di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate, to improve dispersive property.
Starch sizing of the present invention is to take cation cassava starch to be polymerized as main raw material.Before this cation cassava starch was dissolved into to sizing material, be heated to 90 ℃ of-95 ℃ of lower gelatinizations, carry out " liquefaction " effect with α type amylase, а in the hydrolyzed starch molecule-1.4 glucoside bond, generate short chain dextrin and a small amount of low-molecular-weight carbohydrate, add again acrylamide solution (40%), add dimethyl diallyl ammonium chloride to carry out polymerization, with ammonium persulfate, make initator, then adjust the pH value with glacial acetic acid, add shitosan polymerization again, to improve retention performance.
Aluminum sulfate solution of the present invention is without the solution of swage aluminum sulfate (alundum (Al2O3) content >=16.5%) in water.The part by weight of described each component is: without swage aluminum sulfate: water=100:150.
Water of the present invention is deionized water.
With existing technology, compare, 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, this is a kind of high molecular dispersant, the performances such as emulsibility, stability and permeability are preferably arranged, make the associating material of alkyl ketene dimer and paraffin be easier to dissolve, disperse.The present invention successfully synthesizes starch sizing, and this is a kind of high molecular retention agents, has improved stability and the sizing efficiency of product.By 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, then add aluminum sulfate solution and dilution water, the modification AKD neutral sizing agent of making.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, prepare 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 Guangxi bright positive biochemical industry Co., Ltd.
1.1.2, NaOH (99%): 7.5 kilograms;
1.1.3, the chloro-2-hydroxypropyl-trimethyl ammonium chloride of 69%3-: 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 to reactor, add oxidized tapioca under stirring, while being heated to 40 ℃, isothermal reaction 30 minutes;
1.2.2, add NaOH (99%), while being heated to 60-65 ℃, isothermal reaction 30 minutes, start to drip the chloro-2-hydroxypropyl-trimethyl ammonium chloride of 69%3-, after be heated to 70 ℃ of-75 ℃ of lower isothermal reactions 3 hours;
1.2.3, add 86.0 kg of water, add glacial acetic acid, add 40% acrylamide solution, then add tert-dodecyl mercaptan, logical nitrogen 30 minutes;
1.2.4, start to drip emulsifying agent (TX-10) solution again, drip N hydroxymethyl acrylamide solution simultaneously, within 30 minutes, drip, drip ammonium persulfate solution simultaneously, within 40 minutes, drip 5/6ths of solution, stay remaining sixth, material was 85 ℃ of-88 ℃ of lower insulation reaction 1 hour;
1.2.5, stay remaining ammonium persulfate solution with within 10 minutes, dripping again, material was 78 ℃ of-82 ℃ of lower insulation reaction 2 hours; Adding 160.0 kilograms, water, add dispersant N, be warming up to 90 ℃, be incubated 30 minutes, be cooled to 50 ℃ and get final product blowing, is this product dispersant special.
1000 kilograms, water, 100 kilograms of carboxymethyl starch, after finishing material, stir 30 minutes, after be warming up to more than 90 ℃, timing insulated and stirred 2 hours, be cooled to 60 ℃ of blowings, crosses 80 mesh sieves and filter to obtain carboxymethyl starch gelatinization sizing material.
2, prepare 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 Guangxi bright positive biochemical industry 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, after adding α type amylase, be heated to 90 ℃ of-95 ℃ of lower isothermal reactions 1 hour;
2.2.2, add 80.0 kg of water, 40% adds acrylamide solution, under stirring, adds dimethyl diallyl ammonium chloride, logical nitrogen drips ammonium persulfate solution 2 hours, while 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 this product.
3, prepare aluminum sulfate solution
In enamel reaction still, feed intake: 400.0 kilograms are added in 600.0 kg of water without swage aluminum sulfate, stir more than 1 hour, till dissolving to the solids overwhelming majority, filter after 100 eye mesh screens.
4, prepare 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 tank 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 stirring, be heated to 85-90 ℃;
4.3, by the alkyl ketene dimer and the paraffin compound that melt, add in the material of emulsify at a high speed tank of 1500r/min, through high speed dispersion, shear 15 minutes, blowing, filter through 80 eye mesh screens, obtains the dispersion and emulsion sizing material;
4.4, the dispersion and emulsion sizing material is passed into to the high pressure homogenizer of 40MPa, the decompression homogeneous, after homogeneous, sizing material passes through plate type heat exchanger, after being quickly cooled to 25-30 ℃, add 200.0 kilograms of dilution waters and 200.0 kilograms of aluminum sulfate solutions, after stirring, through 100 eye mesh screens, filter, be prepared as finished product.
Claims (6)
1. modification AKD neutral sizing agent, it is characterized in that, its preparation method is by dispersant and starch sizing and a certain amount of dilution water, be heated to 80-90 ℃ after mixing, after add again alkyl ketene dimer, paraffin in conjunction with the blend glue stuff generated, the emulsify at a high speed that carries out 1500r/minr between 60-80 ℃ reacts 15 minutes, pass into again the high pressure homogenizer of 40MPa, the decompression homogeneous, after homogeneous, sizing material passes through plate type heat exchanger, carry out fast cooling after, add a certain amount of dilution water and aluminum sulfate solution, be prepared as finished product; Described dispersant is polymerized with various chemical monomers and other chemical material, is that oxidized tapioca is dissolved into to sizing material, adds NaOH to carry out substitution reaction, and drips 69% the chloro-2-hydroxypropyl-trimethyl ammonium chloride of 3-and carry out graft reaction; Add again glacial acetic acid, 40% acrylamide solution, N hydroxymethyl acrylamide solution carries out polymerization, with tert-dodecyl mercaptan, controls molecular weight, with ammonium persulfate, makes initator, then adds di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate, to improve dispersive property; Described starch sizing is to take cation cassava starch to be polymerized as main raw material, before this cation cassava starch was dissolved into to sizing material, be heated to 90 ℃ of-95 ℃ of lower gelatinizations, carry out " liquefaction " effect with α type amylase, а in the hydrolyzed starch molecule-1.4 glucoside bond, generate short chain dextrin and a small amount of low-molecular-weight carbohydrate, add again 40% acrylamide solution, add dimethyl diallyl ammonium chloride to carry out polymerization, make initator with ammonium persulfate, adjust the pH value with glacial acetic acid again, add shitosan polymerization again, to improve retention performance.
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, it is characterized in that: described alkyl ketene dimer is 1840 type alkyl ketene dimers, in synthesis material, the aliphatic acid of 18 carbochain numbers is containing 40%.
4. modification AKD neutral sizing agent according to claim 1, it is characterized in that: described paraffin is No. 58 paraffin wax fully refineds.
5. modification AKD neutral sizing agent according to claim 1 is characterized in that: aluminum sulfate solution is the solution in water without swage aluminum sulfate, and the part by weight of its each component is: without swage aluminum sulfate: water=100:150.
6. modification AKD neutral sizing agent according to claim 1, it is characterized in that: described water is deionized water.
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| CN102337707B true CN102337707B (en) | 2013-12-25 |
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| CN102635037B (en) * | 2012-05-04 | 2014-06-11 | 陕西科技大学 | Preparation method of amphoteric sweet potato starch microcrystalline wax/ AKD (alkyl ketene dimer) neutral /alkaline sizing agent |
| CN102635036B (en) * | 2012-05-04 | 2014-07-02 | 陕西科技大学 | Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
| CN102635028B (en) * | 2012-05-04 | 2014-04-09 | 陕西科技大学 | Preparation method for cation sweet potato starch microcrystalline wax/alkyl ketene dimer (AKD) neutral/basic sizing agent |
| CN102627733B (en) * | 2012-05-04 | 2013-05-15 | 陕西科技大学 | Preparation method of high-activity half-crosslinking amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent |
| CN102635030B (en) * | 2012-05-04 | 2014-04-09 | 陕西科技大学 | Preparation method for cation corn starch alkyl ketene dimer (AKD) neutral/basic sizing agent |
| CN102635029A (en) * | 2012-05-04 | 2012-08-15 | 陕西科技大学 | Preparation method of cation sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
| CN102635026B (en) * | 2012-05-04 | 2014-03-19 | 陕西科技大学 | Preparation method for sizing curing time-free alkyl ketene dimer (AKD) neutral/basic sizing agent |
| CN102660900B (en) * | 2012-05-04 | 2014-01-29 | 陕西科技大学 | Preparation method of amphoteric corn starch microcrystalline wax/AKD (alkyl ketene dimer)/alkaline sizing agent |
| CN102635022B (en) * | 2012-05-04 | 2013-07-24 | 陕西科技大学 | Preparation method of high-activity ceresin/AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
| CN102635031B (en) * | 2012-05-04 | 2014-05-14 | 陕西科技大学 | Preparation method for cation potato starch microcrystalline wax/alkyl ketene dimer (AKD) neutral/basic sizing agent |
| CN102660899B (en) * | 2012-05-04 | 2014-01-29 | 陕西科技大学 | Method for preparing cation potato starch alkyl ketene dimer (AKD) neutral/alkaline sizing agent |
| CN102635027B (en) * | 2012-05-04 | 2014-05-14 | 陕西科技大学 | Preparation method of cation corn starch microcrystalline wax/AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
| CN103410051A (en) * | 2013-07-09 | 2013-11-27 | 上海东升新材料有限公司 | Surface sizing agent emulsion and preparation method for same |
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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 |
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| 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 |
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