CN102493273B - Alkenyl succinic anhydride emulsion sizing agent and its preparation method - Google Patents
Alkenyl succinic anhydride emulsion sizing agent and its preparation method Download PDFInfo
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- CN102493273B CN102493273B CN201110368172.0A CN201110368172A CN102493273B CN 102493273 B CN102493273 B CN 102493273B CN 201110368172 A CN201110368172 A CN 201110368172A CN 102493273 B CN102493273 B CN 102493273B
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Abstract
The invention relates to an alkenyl succinic anhydride emulsion sizing agent which belongs to the papermaking industrial sizing agent technical field, and the sizing agent comprises alkenyl succinic anhydride, hydrophilic nanometer titanium dioxide or hectorite, Al2(OH)2x(SO4)3-x and deionized water. The preparation method comprises the following steps: dispersing the hydrophilic nanometer titanium dioxide or hectorite in deionized water, mixing with polyaluminium sulfate sol, taking the mixture as a water phase, alkenyl succinic anhydride is taking as an oil phase, uniformly mixing the water phase and the oil phase. The present invention has the beneficial effects that no any surfactant are required to add, the prepared alkenyl succinic anhydride emulsion sizing agent has the advantages of good stability and high sizing efficiency.
Description
technical field
The present invention relates to paper industry sizing agent technical field, particularly a kind of Alkenyl succinic anhydride emulsion sizing agent, also relates to the preparation method of described Alkenyl succinic anhydride emulsion sizing agent.
background technology
Therefore paper is mainly comprised of hydrophilic cellulose fibre, and most of paper is usingd water and manufactured paper with pulp as medium, and gives paper certain water repelling property by adding appropriate sizing agent.Paper sizing agent is generally water-fast amphiphilic materials, by the reacting of its hydrophilic radical and cellulose fibre, combination, impels the large molecule of sizing agent directed in paper, and large hydrophobic group directly reduces paper surface energy outwardly, gives paper WATER RESISTANCE.Sizing agent adds in copy paper system mainly with the form of oil-in-water emulsion at present, and in emulsification, reduce the consumption of low-molecular-weight surfactant as far as possible, because low-molecular-weight surfactant not only can improve paper water absorbing properties, reduce the sizing efficiency of sizing agent, its foam producing to paper machine behavior in service with become the quality of paper also all to there is interference effect.
Alkenyl succinic anhydride is one of sizing agent conventional in paper industry, have that reactivity is high, the feature of facile hydrolysis, generally before applying glue, utilize starch or high molecular polymer and the on-the-spot emulsification of a small amount of surfactant, and in Process of Applying Glue, add a small amount of aluminum sulfate, reduce the adverse effect of its hydrolysis to paper WATER RESISTANCE and paper-making process, improve the sizing efficiency of alkenyl succinic anhydride.For further avoiding the adverse effect of surfactant to paper sizing, overcome starch and macromolecule emulsifier consumption is large, the deficiency that emulsion effective solid content is low, Chinese patent ZL 200810017130.0 has disclosed a kind of method of utilizing inorganic nano-particle bentonite and hydrotalcite to stablize alkenyl succinic anhydride, the method is utilized with the hydrotalcite of positive charge with the poly-effect of the bentonitic micro-wadding of negative electrical charge, improve the compatibility of bentonite to alkenyl succinic anhydride, prepared high dense, stable alkenyl succinic anhydride emulsion, avoided the use of surfactant in emulsion process completely, obtained good sizing efficiency.But because the bentonite granularity of wadding a quilt with cotton after gathering is larger, prepared alkenyl succinic anhydride emulsion liquid-drop diameter is larger, and sizing efficiency still awaits further raising.Chinese patent ZL 200910020447.4 has disclosed a kind of method of utilizing bentonite, shitosan to stablize alkenyl succinic anhydride emulsion, the method has first been prepared the stable alkenyl succinic anhydride emulsion of neutral modification bentonite, recycling ammoniacal liquor or other alkaline matters, the molten shitosan of acid is deposited to bentonite surface, improve the compatibility of bentonite to alkenyl succinic anhydride, obtained the alkenyl succinic anhydride emulsion that stability is better, sizing efficiency is higher.Yet adding of last alkaline matter, will inevitably cause the hydrolysis of alkenyl succinic anhydride.
summary of the invention
The low problem of facile hydrolysis, poor stability, sizing efficiency existing in order to solve above alkenyl succinic anhydride sizing agent, the invention provides a kind of good stability, Alkenyl succinic anhydride emulsion sizing agent that sizing efficiency is high.
The present invention is achieved by the following measures:
, contain alkenyl succinic anhydride, hydrophilic nano titanium dioxide or hectorite, Al
2(OH)
2x(SO
4)
3-xand deionized water,
Wherein, alkenyl succinic anhydride involved in the present invention is the various industrial products for paper-making sizing without emulsification that exist with liquid form under normal temperature, with the weight ratio of deionized water be 1:0.9～5, the weight ratio of hydrophilic nano titanium dioxide or hectorite and alkenyl succinic anhydride is 1:6 ~ 50, polyaluminium sulfate involved in the present invention has another name called basic aluminium sulphate, refer to the inorganic polymer of aluminum sulfate prehydrolysis, molecular formula is Al
2(OH)
2x(SO
4)
3-x, x=0.3 ~ 1.8, are equivalent to [OH
-]/[Al
3+]=0.3 ~ 1.8, with Al
2o
3meter, and the weight ratio of nano titanium oxide or hectorite is generally between 1:5 ~ 1:20.
Preferably the weight ratio of alkenyl succinic anhydride and deionized water is 1:1.8～4.45, and the weight ratio of hydrophilic nano titanium dioxide and alkenyl succinic anhydride is 1:6.5～25, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.75 ~ 1.8, with Al
2o
3meter, Al
2(OH)
2x(SO
4)
3-xwith the weight ratio of hydrophilic nano titanium dioxide be 1:7.5 ~ 20.
Preferably the weight ratio of alkenyl succinic anhydride and deionized water is 1:1～3, and the weight ratio of hectorite and alkenyl succinic anhydride is 1:20 ~ 50, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.45 ~ 0.6, with Al
2o
3meter, Al
2(OH)
2x(SO
4)
3-xwith the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:8 ~ 20.
Preferably the weight ratio of alkenyl succinic anhydride and deionized water is 1:1.88, and the weight ratio of hydrophilic nano titanium dioxide and alkenyl succinic anhydride is 1:25, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.75, with Al
2o
3meter, with the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:10.
Preferably the weight ratio of alkenyl succinic anhydride and deionized water is 1:3, and the weight ratio of hectorite and alkenyl succinic anhydride is 1:20, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.45, with Al
2o
3meter, with the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:8.
Hydrophilic nano titanium dioxide involved in the present invention refers to that any primary particle sizes is less than the synthesis of nano titania powder of 100 nm, comprises various industrial nano titanium dioxide products; Hectorite has another name called lithium soap soil, is a kind of synthetic Magnesosilicate product, and ideal structure formula is Na
0.7[(Si
8mg
5.5li
0.3) O
20(OH)
4], thering is discoid grain structure, particle surface is with permanent negative electrical charge, and disk diameter is about 20 ~ 30 nm, and thickness is about 0.92 nm.
The preparation method of described Alkenyl succinic anhydride emulsion sizing agent, hydrophilic nano titanium dioxide or hectorite are dispersed in deionized water, mix with polyaluminium sulfate colloidal sol, as water, alkenyl succinic anhydride, as oil phase, mixes water and get final product with oil phase.
Al in polyaluminium sulfate colloidal sol
2(OH)
2x(SO
4)
3-xcontent be not particularly limited, so long as it is just passable to realize the content of commercial Application, if cause viscosity cannot realize too greatly commercial Application because content is too high, also cannot apply in this invention Al in preferred described polyaluminium sulfate colloidal sol
2(OH)
2x(SO
4)
3-xcontent with Al
2o
3count 5%.
Described polyaluminium sulfate colloidal sol adopts following any method to make:
(1) use ammoniacal liquor as alkali source, sulfate precipitate aluminum obtains amorphous hydroted alumina, by basicity requirement, getting aluminum sulfate is scattered in deionized water, mix with the amorphous hydroted alumina after above-mentioned washing, in 40 ~ 80 ℃ of peptizations 8 ~ 48 hours, obtain polyaluminium sulfate colloidal sol;
(2) use calcium oxide as alkali source, by basicity requirement, directly aluminum sulfate aqueous solution is carried out to part alkalization, after alkalization, at 60 ℃, peptization reacts 12 hours, crosses the byproduct calcium sulfate that filters out formation, obtains polyaluminium sulfate colloidal sol;
(3) utilize ammoniacal liquor as alkali source, by basicity requirement, directly aluminum sulfate aqueous solution carried out to part alkalization, after alkalization at 60 ℃ peptization 5 hours, obtain polyaluminium sulfate colloidal sol.
In the preparation scheme of Alkenyl succinic anhydride emulsion sizing agent involved in the present invention, water is mixed with oil phase, but both under agitation water was added in oil phase, but also under agitation oil phase is added in water, preferred scheme is under agitation water to be added in oil phase.
ASA emulsion involved in the present invention is prepared in scheme, and described mechanical shearing effect can be provided by any stirring and shearing equipment, and shear agitation speed general control is at 1000 ~ 8000 revs/min, mixing time 2～5 minutes.
The invention has the beneficial effects as follows: do not need to add any surfactant, prepared Alkenyl succinic anhydride emulsion sizing agent good stability, sizing efficiency are high.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described, do not form any limitation of the invention.Except separately indicating, all umbers in embodiment all by weight.
Embodiment 1
Get 6 parts of Al
2(SO
4)
218H
2o, is scattered in 10 parts of deionized waters; Separately get the concentrated ammonia liquor of 3.5 parts of concentration 28%, with after 10.5 parts of deionized water dilutions, get 2 parts of weak ammonias and be placed in reactor; Afterwards, the ammoniacal liquor after 16 parts of aluminum sulfate aqueous solutions and 12 parts of dilutions is added drop-wise in reactor simultaneously, after dripping, continues to stir 30 minutes, with deionized water, will precipitate centrifuge washing to pH=8 left and right.Get in addition 4 parts of Al
2(SO
4)
218H
2o is scattered in 8 parts of deionized waters, and mixes with the amorphous hydroted alumina after above-mentioned washing, with deionized water, gross weight is transferred to 30.6 parts, in 40 ℃ of peptizations 48 hours, obtains mass concentration and is about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=1.8.
Get 3 parts of commodity nano titanium oxides (primary particle sizes 25nm, hydrophilic) and be dispersed in 84 parts of deionized waters, add 3 parts of the polyaluminium sulfate colloidal sols of above-mentioned preparation, under the rotating speed of 1000 revs/min, disperse 10 minutes, as water; Take 30 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 3 minutes under the rotating speed of 6000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 25%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 2 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 107 s.
Embodiment 2
Get 0.9 part of basicity 10%(x=0.3) solid commodity polyaluminium sulfate, with deionized water, be diluted to 3 parts, form polyaluminium sulfate colloidal sol; Separately get 2 parts of commodity nano titanium oxides (primary particle sizes 25nm, hydrophilic) and be dispersed in 95 parts of deionized waters, add 3 parts of above-mentioned ready polyaluminium sulfate colloidal sols, under the rotating speed of 1000 revs/min, disperse 10 minutes, as water; Take 25 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 5 minutes under the rotating speed of 1000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 20 %.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 2.5 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 94 s.
Embodiment 3
Get 2.5 parts of Al
2(SO
4)
218H
2o, is scattered in 4.5 parts of deionized waters; Separately get the concentrated ammonia liquor of 1.5 parts of concentration 28%, with after 4.5 parts of deionized water dilutions, get 1 part and be placed in reactor; Afterwards, the ammoniacal liquor after 7 parts of aluminum sulfate aqueous solutions and 5 parts of dilutions is added drop-wise in reactor simultaneously, after dripping, continues to stir 30 minutes, with deionized water, will precipitate centrifuge washing to pH8 left and right.Get in addition 7.5 parts of Al
2(SO
4)
218H
2o is scattered in 10.5 parts of deionized waters, and mixes with the amorphous hydroted alumina after above-mentioned washing, with deionized water, gross weight is transferred to 30.6 parts, in 80 ℃ of peptizations 8 hours, obtains mass concentration and is about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.75.
Get 1 part of commodity nano titanium oxide (primary particle sizes 18 nm, hydrophilic) and be dispersed in 47 parts of deionized waters, add 2 parts of the polyaluminium sulfate colloidal sols of above-mentioned preparation, under the rotating speed of 1000 revs/min, disperse 10 minutes, as water; Take 25 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 3 minutes under the rotating speed of 5000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 33%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 1.5 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure about 60g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 131s.
Embodiment 4
Get 1 part of Al
2(SO
4)
218H
2o, is scattered in 2 parts of deionized waters; Separately get the concentrated ammonia liquor of 0.6 part of concentration 28%, with after 1.8 parts of deionized water dilutions, get 0.4 part and be placed in reactor; Afterwards, the ammoniacal liquor after 3 parts of aluminum sulfate aqueous solutions and 2 parts of dilutions is added drop-wise in reactor simultaneously, after dripping, continues to stir 30 minutes, with deionized water, will precipitate centrifuge washing to pH8 left and right.Get in addition 9 parts of Al
2(SO
4)
218H
2o is scattered in 18 parts of deionized waters, and mixes with the amorphous hydroted alumina after above-mentioned washing, with deionized water, gross weight is transferred to 30.6 parts, in 80 ℃ of peptizations 8 hours, obtains mass concentration and is about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.3.
Get 1 part of commodity nano titanium oxide (primary particle sizes 18 nm, hydrophilic) and be dispersed in 45 parts of deionized waters, add 4 parts of the polyaluminium sulfate colloidal sols of above-mentioned preparation, under the rotating speed of 1000 revs/min, disperse 10 minutes, as water; Take 50 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 2 minutes under the rotating speed of 8000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 50%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 1 part to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 63s.
Embodiment 5
Get 6 parts of Al
2(SO
4)
218H
2o, is scattered in 10 parts of deionized waters, under agitation slowly adds 0.5 part of calcium oxide (CaO), continue to stir after 30 minutes, at 60 ℃, react 12 hours, cross the calcium sulfate that filters out formation, and with distilled water, gross mass is adjusted to 18 parts, obtain mass concentration and be about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.9.
Get 3 parts of commodity nano titanium oxides (primary particle sizes 50 nm, hydrophilic) and be dispersed in 89 parts of deionized waters, add 8 parts of the polyaluminium sulfate colloidal sols of above-mentioned preparation, under the rotating speed of 1000 revs/min, disperse 10 minutes, as water; Take 20 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 4 minutes under the rotating speed of 2000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 16.7%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 3 parts to execute emulsion, stirs minute 2 clocks under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 103s.
Embodiment 6
Get 6 parts of Al
2(SO
4)
218H
2o, is scattered in 10 parts of deionized waters; Separately get the concentrated ammonia liquor of 0.49 part of concentration 28%, with deionized water, be diluted to 2 parts, and be added drop-wise to gradually in aluminum sulfate solution, after dripping, continue to stir 30 minutes, and at 60 ℃ peptization 5 hours, obtain mass concentration and be about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.45.
Get 2.4 parts of commodity nano titanium oxides (primary particle sizes 80nm, hydrophilic) and be dispersed in 44.4 parts of deionized waters, add 3.2 parts of the polyaluminium sulfate colloidal sols of above-mentioned preparation, under the rotating speed of 1000 revs/min, disperse 10 minutes, as water; Take 20 parts of commodity alkenyl succinic anhydrides, join in the water of above-mentioned preparation, utilize emulsify at a high speed shearing equipment stirring and emulsifying 2 minutes under the rotating speed of 3000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 28.6%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 1.75 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 77s.
Embodiment 7
Get 1 part of Al
2(SO
4)
218H
2o, is scattered in 2 parts of deionized waters; Separately get the concentrated ammonia liquor of 0.6 part of concentration 28%, with after 1.8 parts of deionized water dilutions, get 0.4 part and be placed in reactor; Afterwards, the ammoniacal liquor after 3 parts of aluminum sulfate aqueous solutions and 2 parts of dilutions is added drop-wise in reactor simultaneously, after dripping, continues to stir 30 minutes, with deionized water, will precipitate centrifuge washing to pH8 left and right.Get in addition 9 parts of Al
2(SO
4)
218H
2o is scattered in 18 parts of deionized waters, and mixes with the amorphous hydroted alumina after above-mentioned washing, with deionized water, gross weight is transferred to 30.6 parts, in 80 ℃ of peptizations 8 hours, obtains mass concentration and is about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.3.
Get 2 parts of hectorite powder and be added to gradually in 100 parts of deionized waters that are preheated to 80 ℃ under constantly stirring, after being uniformly dispersed, be cooled to room temperature, place after 48 hours, 10 parts of polyaluminium sulfate colloidal sols that add above-mentioned preparation disperse 2 minutes, as water under the rotating speed of 1000 revs/min; Take 20 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 5 minutes under the rotating speed of 1000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 15.4%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 3 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 82s.
Embodiment 8
Get 1.5 parts of Al
2(SO
4)
218H
2o, is scattered in 3 parts of deionized waters; Separately get the concentrated ammonia liquor of 0.9 part of concentration 28%, with after 2.7 parts of deionized water dilutions, get 0.6 part and be placed in reactor; Afterwards, the ammoniacal liquor after 3.5 parts of aluminum sulfate aqueous solutions and 3 parts of dilutions is added drop-wise in reactor simultaneously, after dripping, continues to stir 30 minutes, with deionized water, will precipitate centrifuge washing to pH8 left and right.Get in addition 8.5 parts of Al
2(SO
4)
218H
2o is scattered in 12 parts of deionized waters, and mixes with the amorphous hydroted alumina after above-mentioned washing, with deionized water, gross weight is transferred to 30.6 parts, in 80
oc peptization 8 hours, obtains mass concentration and is about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.45.
Get 1 part of hectorite powder and be added to gradually in 60 parts of deionized waters that are preheated to 80 ℃ under constantly stirring, after being uniformly dispersed, be cooled to room temperature, place after 48 hours, 2.5 parts of polyaluminium sulfate colloidal sols that add above-mentioned preparation disperse 2 minutes, as water under the rotating speed of 1000 revs/min; Take 20 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 3 minutes under the rotating speed of 5000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 24 %.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 2 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 129 s.
Embodiment 9
Get 6 parts of Al
2(SO
4)
218H
2o, is scattered in 10 parts of deionized waters; Separately get the concentrated ammonia liquor of 0.66 part of concentration 28%, with deionized water, be diluted to 2 parts, and be added drop-wise to gradually in aluminum sulfate solution, after dripping, continue to stir 30 minutes, and at 60 ℃ peptization 5 hours, obtain mass concentration and be about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.6.
Get 0.8 part of hectorite powder and be added to gradually in 40 parts of deionized waters that are preheated to 80 ℃ under constantly stirring, after being uniformly dispersed, be cooled to room temperature, place after 48 hours, 0.8 part of the polyaluminium sulfate colloidal sol that adds above-mentioned preparation disperses 2 minutes, as water under the rotating speed of 1000 revs/min; Take 40 parts of commodity alkenyl succinic anhydrides, the water of above-mentioned preparation is added in alkenyl succinic anhydride, utilize emulsify at a high speed shearing equipment stirring and emulsifying 2 minutes under the rotating speed of 8000 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 49 %.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 1 part to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 107 s.
Embodiment 10
Get 6 parts of Al
2(SO
4)
218H
2o, is scattered in 10 parts of deionized waters, under agitation slowly adds 0.5 part of calcium oxide (CaO), continue to stir after 30 minutes, at 60 ℃, react 12 hours, cross the calcium sulfate that filters out formation, and with distilled water, gross mass is adjusted to 18 parts, obtain mass concentration and be about 5%(by Al
2o
3meter), [OH
-]/[Al
3+the polyaluminium sulfate colloidal sol of]=0.9.
Get 1 part of hectorite powder and be added to gradually in 60 parts of deionized waters that are preheated to 80 ℃ under constantly stirring, after being uniformly dispersed, be cooled to room temperature, place after 48 hours, 1.6 parts of polyaluminium sulfate colloidal sols that add above-mentioned preparation disperse 2 minutes, as water under the rotating speed of 1000 revs/min; Take 30 parts of commodity alkenyl succinic anhydrides, join in the water of above-mentioned preparation, utilize emulsify at a high speed shearing equipment stirring and emulsifying 3 minutes under the rotating speed of 2500 revs/min, make oil-in-water type alkenyl succinic anhydride emulsion stable, homogeneous, in emulsion, the mass percent of alkenyl succinic anhydride is about 32.4%.
Get 100 parts of beating degrees and be about 45
othe poplar BTMP of SR adds in 9900 parts of water, after defiberizing machine is discongested, adds the alkenyl succinic anhydride of above-mentioned 1.5 parts to execute emulsion, stirs 2 minutes under the speed of 750 revs/min, after mixing, adds 2 parts of Al with paper stock
2(SO
4)
218H
2o, and by quick kayser method sheet forming apparatus, copy formulation and measure approximately 60 g/m
2handsheet, and after 105 ℃ of dry 10min, utilizing Liquid Penetrant method (GB/T5405-2002) to record handsheet degree of sizing is 81 s.
Claims (8)
1. an Alkenyl succinic anhydride emulsion sizing agent, is characterized in that containing alkenyl succinic anhydride, hydrophilic nano titanium dioxide or hectorite, Al
2(OH)
2x(SO
4)
3-xand deionized water, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.3 ~ 1.8, wherein, the weight ratio of alkenyl succinic anhydride and deionized water is 1:0.9～5, the weight ratio of hydrophilic nano titanium dioxide or hectorite and alkenyl succinic anhydride is 1:6 ~ 50, with Al
2o
3meter, Al
2(OH)
2x(SO
4)
3-xwith the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:5 ~ 20;
By following steps, obtain:
Hydrophilic nano titanium dioxide or hectorite are dispersed in deionized water, mix with polyaluminium sulfate colloidal sol, as water, alkenyl succinic anhydride, as oil phase, mixes water and get final product with oil phase;
Described polyaluminium sulfate colloidal sol adopts following any method to make:
(1) use ammoniacal liquor as alkali source, sulfate precipitate aluminum obtains amorphous hydroted alumina, by basicity requirement, getting aluminum sulfate is scattered in deionized water, mix with the amorphous hydroted alumina after above-mentioned washing, in 40 ~ 80 ℃ of peptizations 8 ~ 48 hours, obtain polyaluminium sulfate colloidal sol;
(2) will by basicity requirement, directly to aluminum sulfate aqueous solution, carry out part alkalization with calcium oxide as alkali source, after alkalization, at 60 ℃, react 12 hours, cross the byproduct calcium sulfate that filters out formation, obtain polyaluminium sulfate colloidal sol;
(3) utilize ammoniacal liquor as alkali source, by basicity requirement, directly aluminum sulfate aqueous solution carried out to part alkalization, after alkalization at 60 ℃ peptization 5 hours, obtain polyaluminium sulfate colloidal sol.
2. Alkenyl succinic anhydride emulsion sizing agent according to claim 1, the weight ratio that it is characterized in that alkenyl succinic anhydride and deionized water is 1:1.8～4.45, the weight ratio of hydrophilic nano titanium dioxide and alkenyl succinic anhydride is 1:6.5～25, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.75 ~ 1.8, with Al
2o
3meter, Al
2(OH)
2x(SO
4)
3-xwith the weight ratio of hydrophilic nano titanium dioxide be 1:7.5 ~ 20.
3. Alkenyl succinic anhydride emulsion sizing agent according to claim 1, the weight ratio that it is characterized in that alkenyl succinic anhydride and deionized water is 1:1～3, the weight ratio of hectorite and alkenyl succinic anhydride is 1:20 ~ 50, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.45 ~ 0.6, with Al
2o
3meter, Al
2(OH)
2x(SO
4)
3-xwith the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:8 ~ 20.
4. Alkenyl succinic anhydride emulsion sizing agent according to claim 2, the weight ratio that it is characterized in that alkenyl succinic anhydride and deionized water is 1:1.88, the weight ratio of hydrophilic nano titanium dioxide and alkenyl succinic anhydride is 1:25, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.75, with Al
2o
3meter, with the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:10.
5. Alkenyl succinic anhydride emulsion sizing agent according to claim 3, the weight ratio that it is characterized in that alkenyl succinic anhydride and deionized water is 1:3, the weight ratio of hectorite and alkenyl succinic anhydride is 1:20, Al
2(OH)
2x(SO
4)
3-xmiddle x=0.45, with Al
2o
3meter, with the weight ratio of hydrophilic nano titanium dioxide or hectorite be 1:8.
6. Alkenyl succinic anhydride emulsion sizing agent according to claim 1, is characterized in that hydrophilic nano titanium dioxide primary particle sizes is less than 100 nm, and hectorite disk diameter is 20 ~ 30 nm, and thickness is 0.92 nm.
7. Alkenyl succinic anhydride emulsion sizing agent according to claim 1, is characterized in that Al in described polyaluminium sulfate colloidal sol
2(OH)
2x(SO
4)
3-xcontent be 5%.
8. Alkenyl succinic anhydride emulsion sizing agent according to claim 1, it is characterized in that water to mix with oil phase, but both under agitation water was added in oil phase, but also under agitation oil phase is added in water, mixing speed is 1000 ~ 8000 revs/min, mixing time 2～5 minutes.
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