CN102627734B - Preparation method of amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent without sizing lag - Google Patents
Preparation method of amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent without sizing lag Download PDFInfo
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Abstract
Provided is a preparation method of an amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent without sizing lag. The preparation method comprises firstly performing degradation on cassava starch under the effect of fungus alpha-amylase, then enabling the degraded cassava starch to perform cationization with 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride under the effect of sodium hydroxide, and then utilizing acetic acid to achieve neutralization to obtain cation cassava starch solution, enabling the cation cassava starch solution to perform graft copolymerization with vinyl acetate, butyl acrylate, methyl dodecyl acrylate, acrylic acid and vinylcarbinol to obtain a copolymer which is a sizing agent with excellent performance and serves as an emulsifying agent to be applied to emulsification of AKD and beewax to obtain the amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent without the sizing lag. The prepared neutral/alkaline sizing agent emulsion is small in viscosity and good in stability, and emulsion particles are provided with positive charge and negative charge. In addition, half-crosslinking groups are contained in molecules to facilitate retention and tight combination with paper fibers with negative charge. Therefore, the sizing performance is improved, the sizing effect is obvious, and sizing lag does not occur.
Description
Technical field
The invention belongs to polymer chemistry sizing agent technical field, particularly a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent.
Background technology
The major progress of modern applying glue technology be in/popularization of alkaline bleach liquor sizing technology, during acid papermaking is converted into/alkaline paper-making is the great change on world's papermaking history.In/alkaline bleach liquor sizing is in papermaking process, the pH value is adjusted to more than 7, in principle without a kind of glue applying method of Tai-Ace S 150.In commonly used/alkaline sizing agent alkyl ketene dimer (being called for short AKD) is the product of phase late 1940s research and development, AKD be a kind of can with the response type of fibrin reaction in/alkaline sizing agent, it can be as internal sizing agent, again can be as Surface Size.Its constructional feature is to be made of active group and hydrophobic grouping, the fusing point of AKD is lower, active group quaternary lactonic ring energy under the hot conditions of Dryer Section of Paper Machine in molecule and the hydroxyl reaction on Mierocrystalline cellulose form the beta-keto ester bond and are positioned on fiber, and the hydrophobic group chain alkyl produces the water resistant effect at fiber surface.By in AKD/alkaline bleach liquor sizing, the one way retention of Paper White Degree, feel, water resisting property, physical strength, printability, ageing resistance and filler etc. all is significantly improved.And can to adopt cheap water-ground limestone be filler, reduced the content of objectionable impurities in plain boiled water, improved the cyclic utilization rate of plain boiled water, and AKD is lower than the cost of acid accumulator size simultaneously.Adopt AKD carry out in/alkaline bleach liquor sizing can improve paper product quality and price, reduction energy consumption, improve environmental pollution and paper machine operation performance etc., therefore can obtain obvious economic benefit and social benefit, increasing papermaking enterprise is recognized and is used in AKD/superiority and the necessity of alkaline sizing agent.China's paper making raw material is take straw pulp as main, timber resource shortage, and the secondary stock consumption increases, in utilization/the alkaline bleach liquor sizing technology has realistic meaning.Follow in AKD/the alkaline bleach liquor sizing technology progressively enlarges in China's Application Areas, Technology is increasingly mature, in/benefit of alkaline paper-making progressively embodied, accelerated paper industry by acid papermaking in/trend that alkaline paper-making changes, in recent years AKD become domestic paper plant use at most, the most ripe, the most effective in/alkaline sizing agent.
In AKD/alkaline bleach liquor sizing gives paper some excellent properties, and its weak point is also arranged simultaneously.The reaction of AKD and paper fibre can continue to carry out within a certain period of time, and the AKD applying glue is not yet completed after page is done, and is still carrying out after batching, and is also carrying out in some weeks even thereafter in 24 hours.Along with the prolongation of shelf-time, the degree of sizing of page can rise, therefore under paper roll, machine just can reach best sizing efficiency after for some time.Be prone to during this period the phenomenon that sizing efficiency goes down, and the strength property of sized paper decreases.Improve in recent years and to improve the research of AKD emulsion property increasingly active, alleviate or eliminate the phenomenon that AKD emulsion sizing efficiency goes down, it is that China's papermaking researcher is made great efforts the problem studied always that development and production arrives the short and stable AKD emulsion of sizability of time of best sizing efficiency.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, in gained/alkaline sizing agent has good stability, it is stable that the water repelling property of lower machine after dryer sizing paper and strength property keep, and eliminated the phenomenon that AKD emulsion sizing efficiency goes down.
For achieving the above object, the technical solution used in the present invention is:
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, comprise following concrete steps:
the first step, with water, tapioca (flour) and fungal alpha-amylase added in the first reactor in the time of 50-55 ℃ reaction 1.0-2.0 hour, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add sodium hydroxide, be warmed up to 60-70 ℃ and add the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, be warming up to again 90-95 ℃ of reaction 1.0-2.0 hour, be cooled to 50-55 ℃ and add acetic acid, be down to again 20-30 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with vinyl acetate, ethyl propenoate, methacrylic dodecyl gallate, vinylformic acid and vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, ammonium persulphate and water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add cation cassava starch solution and water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 60-70 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.0-2.0 hour
The 5th step, reinforced complete rear in 80-90 ℃ of insulation reaction 2.0-3.0 hour,
The 6th step cooled to 30-40 ℃, and with 100-200 order net filtration, discharging obtains the AKD emulsifying agent,
The 7th step, add AKD emulsifying agent, beeswax and AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 80-85 ℃, after beeswax and AKD melting, stirred 30-40 minute, under agitation add the hot water of 80-85 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 25-30MPa homogeneous, be cooled to 25-30 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 60-65 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 2.5-3.0 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 32-37 gram/rice
2, ring crush index is 7.5-8.0 ox rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 30-35 gram/rice
2, ring crush index is 7.4-7.9 ox rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 30-35 gram/rice
2, ring crush index is 7.4-7.9 ox rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 29-34 gram/rice
2, ring crush index is 7.3-7.8 ox rice
2The applying glue hysteresis phenomenon does not appear in/gram.
Do not use the small molecules tensio-active agent in preparation process of the present invention, be conducive to the raising of environment protection and effect.First then the tapioca (flour) degraded is carried out cationization, carry out graft copolymerization with acrylate again, the multipolymer that obtains itself is exactly the sizing agent of excellent performance, it is applied to the emulsification of AKD and beeswax as emulsifying agent, in preparation/the alkaline sizing agent emulsion viscosity is little, good stability, emulsion particle is with positive charge and negative charge, contain again simultaneously half crosslinking structure, help to keep and can combine closely with electronegative paper fibre, therefore greatly improved sizability, sizing efficiency is obvious, the applying glue hysteresis phenomenon do not occur.
Embodiment
The below will the present invention is described in further detail with specific embodiment.
Embodiment one
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, specifically comprise the following steps:
the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 50 ℃ reaction 1.0 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 60 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 90 ℃ of reactions 2.0 hours, be cooled to 50 ℃ and add 7 gram acetic acid, be down to again 20 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 60 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.0 hours
The 5th step, reinforced complete after in 80 ℃ of insulation reaction 3.0 hours,
The 6th step cooled to 30 ℃, and with 100 order net filtrations, discharging obtains the AKD emulsifying agent,
The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 80 ℃, after beeswax and AKD melting, stirred 30 minutes, under agitation add the hot water of 80 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 25MPa homogeneous, be cooled to 25 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 60 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 2.5 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 37 gram/rice
2, ring crush index is 7.5 Ns of rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 35 gram/rice
2, ring crush index is 7.4 Ns of rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 35 gram/rice
2, ring crush index is 7.4 Ns of rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 34 gram/rice
2, ring crush index is 7.3 Ns of rice
2The applying glue hysteresis phenomenon does not appear in/gram.
Embodiment two
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, specifically comprise the following steps:
the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 51 ℃ reaction 1.2 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 62 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 91 ℃ of reactions 1.8 hours, be cooled to 51 ℃ and add 7 gram acetic acid, be down to again 22 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 62 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.2 hours
The 5th step, reinforced complete after in 82 ℃ of insulation reaction 2.8 hours,
The 6th step cooled to 32 ℃, and with 120 order net filtrations, discharging obtains the AKD emulsifying agent,
The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 81 ℃, after beeswax and AKD melting, stirred 32 minutes, under agitation add the hot water of 81 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 26MPa homogeneous, be cooled to 26 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 61 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 2.6 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 36 gram/rice
2, ring crush index is 7.6 Ns of rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 34 gram/rice
2, ring crush index is 7.5 Ns of rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 34 gram/rice
2, ring crush index is 7.5 Ns of rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 33 gram/rice
2, ring crush index is 7.4 Ns of rice
2The applying glue hysteresis phenomenon does not appear in/gram.
Embodiment three
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, specifically comprise the following steps:
the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 52 ℃ reaction 1.4 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 64 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 92 ℃ of reactions 1.6 hours, be cooled to 52 ℃ and add 7 gram acetic acid, be down to again 24 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 64 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.4 hours
The 5th step, reinforced complete after in 84 ℃ of insulation reaction 2.6 hours,
The 6th step cooled to 34 ℃, and with 140 order net filtrations, discharging obtains the AKD emulsifying agent,
The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 82 ℃, after beeswax and AKD melting, stirred 34 minutes, under agitation add the hot water of 82 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 27MPa homogeneous, be cooled to 27 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 62 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 2.7 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 35 gram/rice
2, ring crush index is 7.7 Ns of rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 33 gram/rice
2, ring crush index is 7.6 Ns of rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 33 gram/rice
2, ring crush index is 7.6 Ns of rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 32 gram/rice
2, ring crush index is 7.5 Ns of rice
2The applying glue hysteresis phenomenon does not appear in/gram.
Embodiment four
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, specifically comprise the following steps:
the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 53 ℃ reaction 1.6 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 66 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 93 ℃ of reactions 1.4 hours, be cooled to 53 ℃ and add 7 gram acetic acid, be down to again 26 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 66 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.6 hours
The 5th step, reinforced complete after in 86 ℃ of insulation reaction 2.4 hours,
The 6th step cooled to 36 ℃, and with 160 order net filtrations, discharging obtains the AKD emulsifying agent,
The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 83 ℃, after beeswax and AKD melting, stirred 36 minutes, under agitation add the hot water of 83 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 28MPa homogeneous, be cooled to 28 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 63 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 2.8 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 34 gram/rice
2, ring crush index is 7.8 Ns of rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 32 gram/rice
2, ring crush index is 7.7 Ns of rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 32 gram/rice
2, ring crush index is 7.7 Ns of rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 31 gram/rice
2, ring crush index is 7.6 Ns of rice
2The applying glue hysteresis phenomenon does not appear in/gram.
Embodiment five
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, specifically comprise the following steps:
the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 54 ℃ reaction 1.8 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 68 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 94 ℃ of reactions 1.2 hours, be cooled to 54 ℃ and add 7 gram acetic acid, be down to again 28 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 68 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.8 hours
The 5th step, reinforced complete after in 88 ℃ of insulation reaction 2.2 hours,
The 6th step cooled to 38 ℃, and with 180 order net filtrations, discharging obtains the AKD emulsifying agent,
The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 84 ℃, after beeswax and AKD melting, stirred 38 minutes, under agitation add the hot water of 84 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 29MPa homogeneous, be cooled to 29 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 64 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 2.9 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 33 gram/rice
2, ring crush index is 7.9 Ns of rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 31 gram/rice
2, ring crush index is 7.8 Ns of rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 31 gram/rice
2, ring crush index is 7.8 Ns of rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 30 gram/rice
2, ring crush index is 7.7 Ns of rice
2The applying glue hysteresis phenomenon does not appear in/gram.
Embodiment six
A kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, specifically comprise the following steps:
the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 55 ℃ reaction 2.0 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 70 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 95 ℃ of reactions 1.0 hours, be cooled to 55 ℃ and add 7 gram acetic acid, be down to again 30 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,
Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,
The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,
The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 70 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 2.0 hours
The 5th step, reinforced complete after in 90 ℃ of insulation reaction 2.0 hours,
The 6th step cooled to 40 ℃, and with 200 order net filtrations, discharging obtains the AKD emulsifying agent,
The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 85 ℃, after beeswax and AKD melting, stirred 40 minutes, under agitation add the hot water of 85 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 30MPa homogeneous, be cooled to 30 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
With this without in applying glue hysteresis both sexes AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the Corrugating Base Paper top sizing, starch consumption 65 kg/ton paper, without in applying glue hysteresis both sexes AKD/alkaline sizing agent 3.0 kg/ton paper, the Cobb value of lower machine after dryer sizing Corrugating Base Paper is 32 gram/rice
2, ring crush index is 8.0 Ns of rice
2/ gram; The Cobb value of 2 hours after dryer sizing Corrugating Base Papers is 30 gram/rice
2, ring crush index is 7.9 Ns of rice
2/ gram; The Cobb value of 24 hours after dryer sizing Corrugating Base Papers is 30 gram/rice
2, ring crush index is 7.9 Ns of rice
2/ gram; The Cobb value of 7 days after dryer sizing Corrugating Base Papers is 29 gram/rice
2, ring crush index is 7.8 Ns of rice
2The applying glue hysteresis phenomenon does not appear in/gram.
in sum, the invention gained a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, carry out cationization after adopting the tapioca (flour) degraded, carry out graft copolymerization with acrylate again, the multipolymer that obtains itself is exactly the sizing agent of excellent performance, it is applied to the emulsification of AKD and beeswax as emulsifying agent, in preparation/the alkaline sizing agent emulsion viscosity is little, good stability, emulsion particle is with positive charge and negative charge, contain again half crosslinked group in molecule, help to keep and can combine closely with electronegative paper fibre, therefore greatly improved sizability, sizing efficiency is obvious, the applying glue hysteresis phenomenon does not appear.
Claims (7)
- One kind without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, comprise following concrete steps:the first step, with water, tapioca (flour) and fungal alpha-amylase added in the first reactor in the time of 50-55 ℃ reaction 1.0-2.0 hour, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add sodium hydroxide, be warmed up to 60-70 ℃ and add the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, be warming up to again 90-95 ℃ of reaction 1.0-2.0 hour, be cooled to 50-55 ℃ and add acetic acid, be down to again 20-30 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with vinyl acetate, ethyl propenoate, methacrylic dodecyl gallate, vinylformic acid and vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, ammonium persulphate and water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add cation cassava starch solution and water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 60-70 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.0-2.0 hourThe 5th step, reinforced complete rear in 80-90 ℃ of insulation reaction 2.0-3.0 hour,The 6th step cooled to 30-40 ℃, and with 100-200 order net filtration, discharging obtains the AKD emulsifying agent,The 7th step, add AKD emulsifying agent, beeswax and AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 80-85 ℃, after beeswax and AKD melting, stirred 30-40 minute, under agitation add the hot water of 80-85 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 25-30MPa homogeneous, be cooled to 25-30 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
- According to claim 1 a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, specifically comprise the following steps:the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 50 ℃ reaction 1.0 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 60 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 90 ℃ of reactions 2.0 hours, be cooled to 50 ℃ and add 7 gram acetic acid, be down to again 20 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 60 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.0 hoursThe 5th step, reinforced complete after in 80 ℃ of insulation reaction 3.0 hours,The 6th step cooled to 30 ℃, and with 100 order net filtrations, discharging obtains the AKD emulsifying agent,The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 80 ℃, after beeswax and AKD melting, stirred 30 minutes, under agitation add the hot water of 80 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 25MPa homogeneous, be cooled to 25 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
- According to claim 1 a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, specifically comprise the following steps:the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 51 ℃ reaction 1.2 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 62 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 91 ℃ of reactions 1.8 hours, be cooled to 51 ℃ and add 7 gram acetic acid, be down to again 22 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 62 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.2 hoursThe 5th step, reinforced complete after in 82 ℃ of insulation reaction 2.8 hours,The 6th step cooled to 32 ℃, and with 120 order net filtrations, discharging obtains the AKD emulsifying agent,The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 81 ℃, after beeswax and AKD melting, stirred 32 minutes, under agitation add the hot water of 81 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 26MPa homogeneous, be cooled to 26 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
- According to claim 1 a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, specifically comprise the following steps:the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 52 ℃ reaction 1.4 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 64 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 92 ℃ of reactions 1.6 hours, be cooled to 52 ℃ and add 7 gram acetic acid, be down to again 24 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 64 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.4 hoursThe 5th step, reinforced complete after in 84 ℃ of insulation reaction 2.6 hours,The 6th step cooled to 34 ℃, and with 140 order net filtrations, discharging obtains the AKD emulsifying agent,The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 82 ℃, after beeswax and AKD melting, stirred 34 minutes, under agitation add the hot water of 82 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 27MPa homogeneous, be cooled to 27 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
- According to claim 1 a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, specifically comprise the following steps:the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 53 ℃ reaction 1.6 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 66 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 93 ℃ of reactions 1.4 hours, be cooled to 53 ℃ and add 7 gram acetic acid, be down to again 26 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 66 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.6 hoursThe 5th step, reinforced complete after in 86 ℃ of insulation reaction 2.4 hours,The 6th step cooled to 36 ℃, and with 160 order net filtrations, discharging obtains the AKD emulsifying agent,The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 83 ℃, after beeswax and AKD melting, stirred 36 minutes, under agitation add the hot water of 83 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 28MPa homogeneous, be cooled to 28 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
- According to claim 1 a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, specifically comprise the following steps:the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 54 ℃ reaction 1.8 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 68 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 94 ℃ of reactions 1.2 hours, be cooled to 54 ℃ and add 7 gram acetic acid, be down to again 28 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 68 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 1.8 hoursThe 5th step, reinforced complete after in 88 ℃ of insulation reaction 2.2 hours,The 6th step cooled to 38 ℃, and with 180 order net filtrations, discharging obtains the AKD emulsifying agent,The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 84 ℃, after beeswax and AKD melting, stirred 38 minutes, under agitation add the hot water of 84 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 29MPa homogeneous, be cooled to 29 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
- According to claim 1 a kind of without in applying glue hysteresis both sexes AKD/preparation method of alkaline sizing agent, it is characterized in that, specifically comprise the following steps:the first step, with 200 gram water, 100 gram tapioca (flour)s and 0.6 gram fungal alpha-amylase added in the first reactor in the time of 55 ℃ reaction 2.0 hours, obtain degrading cassava starch, water, the mass ratio of tapioca (flour) and fungal alpha-amylase is 200: 100: 0.6, then add 10 gram sodium hydroxide, be warmed up to 70 ℃ and add 70 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, be warming up to again 95 ℃ of reactions 1.0 hours, be cooled to 55 ℃ and add 7 gram acetic acid, be down to again 30 ℃, tapioca (flour), sodium hydroxide, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 10: 70: 7, add water adjusting solid content to 25% in the first reactor, namely get cation cassava starch solution,Second step, with 18 gram vinyl acetates, 10 gram ethyl propenoates, 7 gram methacrylic dodecyl gallates, 4 gram vinylformic acid and 1 gram vinylcarbinol by 18: 10: 7: the mass ratio of 4: 1 is mixed and made into mix monomer,The 3rd step, 1 gram ammonium persulphate and 20 gram water are made ammonium persulfate aqueous solution with mass ratio at 1: 20,The 4th step, add 80 gram cation cassava starch solution and 99 gram water in the second reactor, the mass ratio of cation cassava starch solution and water is 80: 99, be warming up to 70 ℃, add simultaneously ammonium persulfate aqueous solution and mix monomer, the mass ratio of cation cassava starch solution, ammonium persulfate aqueous solution and mix monomer is 80: 21: 40, and whole feed time is 2.0 hoursThe 5th step, reinforced complete after in 90 ℃ of insulation reaction 2.0 hours,The 6th step cooled to 40 ℃, and with 200 order net filtrations, discharging obtains the AKD emulsifying agent,The 7th step, add 110 gram AKD emulsifying agents, 80 gram beeswaxs and 150 gram AKD in the 3rd reactor, wherein the mass ratio of AKD emulsifying agent, beeswax and AKD is 110: 80: 150, be warming up to 85 ℃, after beeswax and AKD melting, stirred 40 minutes, under agitation add the hot water of 85 ℃ to regulate solid content to 15%, make cation cassava starch AKD meta emulsion, with the meta emulsion after the 30MPa homogeneous, be cooled to 30 ℃, obtain solid content and be 15% stable without in applying glue hysteresis both sexes AKD/alkaline sizing agent.
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