CN114960279B - AKD production process based on dopamine modified titanium dioxide - Google Patents
AKD production process based on dopamine modified titanium dioxide Download PDFInfo
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Abstract
The invention relates to the technical field of AKD (alkyl ketene dimer) emulsification technology, and provides an AKD production technology based on dopamine modified titanium dioxide, wherein the titanium dioxide is modified by the dopamine, so that the titanium dioxide has higher adhesion, an interfacial film can be formed at an oil-water interface, so that interfacial tension and interfacial energy are reduced, liquid drop coalescence is prevented, and the stability of emulsion after AKD emulsification can be improved to a certain extent; the high-cationic acrylic ester polymer is added in the process of preparing the composite cationic starch emulsifier, and a supermolecule composite system can be formed in the composite cationic starch emulsifier through static electricity, hydrogen bonds and other acting forces of different components, so that the emulsifying property of the corn starch is improved; according to the invention, the AKD is modified by the polyethyleneimine, and the hydrophilic parent group in the polyethyleneimine can improve the adhesion rate of emulsion particles on the fiber, so that the stability and the retention rate of the AKD emulsion can be improved.
Description
Technical Field
The invention relates to the technical field of AKD emulsification processes, in particular to an AKD production process based on dopamine modified titanium dioxide.
Background
In recent years, as the price of rosin is continuously increased, the cost of traditional rosin sizing is also increased, and the AKD neutral sizing is also attracting more and more attention. AKD sizing agents are difficult to retain on the fibers during use because AKD is itself uncharged, and generally require emulsification of AKD using cationic emulsifiers to positively charge the AKD and adsorb to negatively charged fibers.
Cationic starch is generally used as an emulsifier of AKD in the early stage, but the cationic starch has lower charge density, higher molecular mass and lower bonding strength with AKD particles, so that the emulsion has poorer stability and sizing effect; in addition, starch is easy to mold and can cause emulsion deterioration, so how to design an AKD emulsifying process to ensure that AKD prepared by emulsification has better stability and high retention rate becomes a technical problem to be solved by the technicians in the field.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an AKD production process based on dopamine modified titanium dioxide, which aims at ensuring that AKD emulsion prepared by emulsification has better stability and high retention rate.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme:
an AKD production process based on dopamine modified titanium dioxide comprises the following production steps:
s1, weighing 40 parts of sodium hydroxide, placing the sodium hydroxide into a beaker, adding 1000ml of deionized water, uniformly stirring, heating to 35-40 ℃, weighing a proper amount of dopamine, adding the dopamine into the beaker, stirring, weighing a proper amount of titanium dioxide, adding the titanium dioxide into the beaker, reacting for a period of time under the condition of keeping the temperature unchanged, finally carrying out suction filtration on the product, washing the product for a plurality of times by using the deionized water, placing the washed product into a 60 ℃ oven for drying, and grinding the dried product to obtain the dopamine-modified titanium dioxide;
s2, according to 10:1, mixing the composite cationic starch emulsifier and the compound emulsifier in a mass ratio, and uniformly mixing to obtain a mixed emulsifier;
s3, heating and melting AKD wax powder in a water bath, slowly adding the preheated polyethyleneimine solution into the melted AKD after the AKD is completely melted, adding a proper amount of deionized water after high-speed shearing and stirring for 1min, continuing high-speed shearing and stirring for 10min, standing for 1h, and cooling to normal temperature to obtain the polyethyleneimine modified AKD;
s4, weighing 200 parts of AKD modified by polyethyleneimine in S3 and a proper amount of deionized water, adding into a three-neck flask, stirring, heating at 60 ℃ until the AKD is completely melted, adding 8-10 parts of titanium dioxide modified by dopamine in S1 and 16-20 parts of mixed emulsifier in S2 after increasing the rotating speed, premixing for 5min, and transferring into a homogenizer;
s5, adding a dispersing agent and a synergistic agent into the system of the homogenizer in S4, shearing and emulsifying for 10-20min at a high speed of 10000r/min by using a high-shearing emulsifying machine after uniformly mixing, cooling to room temperature, and adding 13-15 parts of polyaluminium chloride and uniformly mixing to obtain the AKD emulsion.
Further, the mass ratio of dopamine to titanium dioxide in the S1 is 3:2.
further, the stirring rotation speed in the step S1 is 500r/min.
Further, the preparation method of the composite cationic starch emulsifier in the step S2 comprises the following steps:
step 1: adding 50 parts of corn starch, 1-2 parts of ammonium persulfate, 1-2 parts of cross-linking agent and 3-4 parts of high-positive-charge acrylic ester polymer into a flask, and gelatinizing for 30min at 95 ℃;
step 2: adding a proper amount of deionized water into the system in the step 1 for dilution, and then adjusting the pH value to 3 by using acetic acid to obtain the composite cationic starch emulsifier.
Further, the preparation method of the compound emulsifier in the step S2 comprises the following steps:
step one: weighing 2 parts of nonionic surfactant and 1 part of cationic surfactant, pouring into a beaker, adding a proper amount of solvent, and mixing and stirring;
step two: and (3) uniformly stirring the system in the step one, and then performing ultrasonic dispersion for 15min at the frequency of 10000-12000Hz to obtain the compound emulsifier.
Further, the water bath temperature in the step S3 is 70-80 ℃.
Further, the stirring speed in the step S4 is 300-500r/min.
Still further, the dispersant in S5 is hexenyl bis stearamide.
Still further, the synergist in S5 is modified guar gum powder.
Further, the preparation method of the modified guar gum comprises the following steps: adding alkali liquor into a reaction kettle, adding guar gum powder under the stirring condition of 300-400rpm, adding galactose oxidase and mannase when the stirring speed is increased to 600-800rpm, uniformly dispersing, reacting for 3-4 hours at 120-130 ℃, pouring the obtained product into an ethanol water solution to adjust the pH value to 7, filtering out supernatant, washing the precipitate by using the ethanol water solution, and drying and crushing to obtain the modified guar gum powder.
Advantageous effects
Compared with the prior art, the AKD production process based on the dopamine modified titanium dioxide has the following beneficial effects:
according to the invention, the titanium dioxide is modified by the dopamine, so that the titanium dioxide has higher adhesion, and an interfacial film can be formed at an oil-water interface, so that the interfacial tension and the interfacial energy are reduced, the coalescence of liquid drops is prevented, and the stability of emulsion after AKD emulsification can be improved to a certain extent; the high-positive-charge acrylic ester polymer is added in the process of preparing the composite cationic starch emulsifier, and a supermolecule composite system can be formed in the composite cationic starch emulsifier through static electricity, hydrogen bonds and other acting forces of different components, so that the emulsifying property of corn starch is improved, and secondly, positive charges carried in the composite cationic starch emulsifier can play a synergistic effect with AKD in the process of AKD sizing, and the retention rate of AKD sizing is improved; according to the invention, the AKD is modified by the polyethyleneimine, and the hydrophilic parent group in the polyethyleneimine can improve the adhesion rate of emulsion particles on the fiber, so that the stability and the retention rate of the AKD emulsion can be improved.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the AKD production process based on the dopamine-modified titanium dioxide of the embodiment comprises the following production steps:
s1, weighing 40 parts of sodium hydroxide, placing the sodium hydroxide into a beaker, adding 1000ml of deionized water, uniformly stirring, heating to 35 ℃, weighing a proper amount of dopamine, adding the dopamine into the beaker, stirring, weighing a proper amount of titanium dioxide, adding the titanium dioxide into the beaker, reacting for a period of time under the condition of keeping the temperature unchanged, finally carrying out suction filtration on the product, washing the product for a plurality of times by using the deionized water, drying the washed product in a 60 ℃ oven, and grinding the dried product to obtain the dopamine-modified titanium dioxide;
s2, according to 10:1, mixing the composite cationic starch emulsifier and the compound emulsifier in a mass ratio, and uniformly mixing to obtain a mixed emulsifier;
s3, heating and melting AKD wax powder in a water bath, slowly adding the preheated polyethyleneimine solution into the melted AKD after the AKD is completely melted, adding a proper amount of deionized water after high-speed shearing and stirring for 1min, continuing high-speed shearing and stirring for 10min, standing for 1h, and cooling to normal temperature to obtain the polyethyleneimine modified AKD;
s4, weighing 200 parts of AKD modified by polyethyleneimine in S3 and a proper amount of deionized water, adding into a three-neck flask, stirring, heating at 60 ℃ until the AKD is completely melted, adding 9 parts of titanium dioxide modified by dopamine in S1 and 18 parts of mixed emulsifier in S2 after increasing the rotating speed, premixing for 5min, and transferring into a homogenizer;
s5, adding a dispersing agent and a synergistic agent into the system of the homogenizer in S4, uniformly mixing, shearing and emulsifying for 10min at a high speed of 10000r/min by using a high-shearing emulsifying machine, cooling to room temperature, adding 15 parts of polyaluminium chloride, and uniformly mixing to obtain the AKD emulsion.
In S1, the mass ratio of dopamine to titanium dioxide is 3:2.
the stirring speed in S1 was 500r/min.
The preparation method of the composite cationic starch emulsifier in S2 comprises the following steps:
step 1: adding 50 parts of corn starch, 1 part of ammonium persulfate, 1 part of cross-linking agent and 4 parts of high-positive-charge acrylic ester polymer into a flask, and gelatinizing for 30min at 95 ℃;
step 2: adding a proper amount of deionized water into the system in the step 1 for dilution, and then adjusting the pH value to 3 by using acetic acid to obtain the composite cationic starch emulsifier.
The preparation method of the compound emulsifier in S2 comprises the following steps:
step one: weighing 2 parts of nonionic surfactant and 1 part of cationic surfactant, pouring into a beaker, adding a proper amount of solvent, and mixing and stirring;
step two: and (3) uniformly stirring the system in the step one, and then, performing ultrasonic dispersion for 15min at the frequency of 11000Hz to obtain the compound emulsifier.
The water bath temperature in S3 was 75 ℃.
The stirring speed and the rotating speed in the step S4 are 300r/min.
The dispersant in S5 is hexenyl bis stearamide.
The synergist in S5 is modified guar gum powder.
The preparation method of the modified guar gum comprises the following steps: adding alkali liquor into a reaction kettle, adding guar gum powder under the stirring condition of 400rpm, adding galactose oxidase and mannase when the stirring speed is increased to 800rpm, uniformly dispersing, reacting for 3 hours at 120 ℃, pouring the obtained product into an ethanol water solution, regulating the pH value to 7, filtering out supernatant, washing the precipitate by using the ethanol water solution, and drying and crushing to obtain modified guar gum powder.
Example 2:
the AKD production process based on the dopamine-modified titanium dioxide of the embodiment comprises the following production steps:
s1, weighing 40 parts of sodium hydroxide, placing the sodium hydroxide into a beaker, adding 1000ml of deionized water, uniformly stirring, heating to 38 ℃, weighing a proper amount of dopamine, adding the dopamine into the beaker, stirring, weighing a proper amount of titanium dioxide, adding the titanium dioxide into the beaker, reacting for a period of time under the condition of keeping the temperature unchanged, finally carrying out suction filtration on the product, washing the product for a plurality of times by using the deionized water, drying the washed product in a 60 ℃ oven, and grinding the dried product to obtain the dopamine-modified titanium dioxide;
s2, according to 10:1, mixing the composite cationic starch emulsifier and the compound emulsifier in a mass ratio, and uniformly mixing to obtain a mixed emulsifier;
s3, heating and melting AKD wax powder in a water bath, slowly adding the preheated polyethyleneimine solution into the melted AKD after the AKD is completely melted, adding a proper amount of deionized water after high-speed shearing and stirring for 1min, continuing high-speed shearing and stirring for 10min, standing for 1h, and cooling to normal temperature to obtain the polyethyleneimine modified AKD;
s4, weighing 200 parts of AKD modified by polyethyleneimine in S3 and a proper amount of deionized water, adding into a three-neck flask, stirring, heating at 60 ℃ until the AKD is completely melted, adding 10 parts of titanium dioxide modified by dopamine in S1 and 16 parts of mixed emulsifier in S2 after increasing the rotating speed, premixing for 5min, and transferring into a homogenizer;
s5, adding a dispersing agent and a synergistic agent into the system of the homogenizer in S4, uniformly mixing, shearing and emulsifying for 20min at a high speed of 10000r/min by using a high-shearing emulsifying machine, cooling to room temperature, and adding 13 parts of polyaluminium chloride, and uniformly mixing to obtain the AKD emulsion.
In S1, the mass ratio of dopamine to titanium dioxide is 3:2.
the stirring speed in S1 was 500r/min.
The preparation method of the composite cationic starch emulsifier in S2 comprises the following steps:
step 1: adding 50 parts of corn starch, 1 part of ammonium persulfate, 2 parts of cross-linking agent and 3 parts of high-positive-charge acrylic ester polymer into a flask, and gelatinizing for 30min at 95 ℃;
step 2: adding a proper amount of deionized water into the system in the step 1 for dilution, and then adjusting the pH value to 3 by using acetic acid to obtain the composite cationic starch emulsifier.
The preparation method of the compound emulsifier in S2 comprises the following steps:
step one: weighing 2 parts of nonionic surfactant and 1 part of cationic surfactant, pouring into a beaker, adding a proper amount of solvent, and mixing and stirring;
step two: and (3) uniformly stirring the system in the step one, and then, performing ultrasonic dispersion for 15min at the frequency of 10000Hz to obtain the compound emulsifier.
The water bath temperature in S3 was 80 ℃.
The stirring speed and the rotating speed in the step S4 are 500r/min.
The dispersant in S5 is hexenyl bis stearamide.
The synergist in S5 is modified guar gum powder.
The preparation method of the modified guar gum comprises the following steps: adding alkali liquor into a reaction kettle, adding guar gum powder under the stirring condition of 300rpm, adding galactose oxidase and mannase when the stirring speed is increased to 700rpm, uniformly dispersing, reacting for 4 hours at 125 ℃, pouring the obtained product into an ethanol water solution, regulating the pH value to 7, filtering out supernatant, washing the precipitate by using the ethanol water solution, and drying and crushing to obtain modified guar gum powder.
Example 3:
the AKD production process based on the dopamine-modified titanium dioxide of the embodiment comprises the following production steps:
s1, weighing 40 parts of sodium hydroxide, placing the sodium hydroxide into a beaker, adding 1000ml of deionized water, uniformly stirring, heating to 40 ℃, weighing a proper amount of dopamine, adding the dopamine into the beaker, stirring, weighing a proper amount of titanium dioxide, adding the titanium dioxide into the beaker, reacting for a period of time under the condition of keeping the temperature unchanged, finally carrying out suction filtration on the product, washing the product for a plurality of times by using the deionized water, drying the washed product in a 60 ℃ oven, and grinding the dried product to obtain the dopamine-modified titanium dioxide;
s2, according to 10:1, mixing the composite cationic starch emulsifier and the compound emulsifier in a mass ratio, and uniformly mixing to obtain a mixed emulsifier;
s3, heating and melting AKD wax powder in a water bath, slowly adding the preheated polyethyleneimine solution into the melted AKD after the AKD is completely melted, adding a proper amount of deionized water after high-speed shearing and stirring for 1min, continuing high-speed shearing and stirring for 10min, standing for 1h, and cooling to normal temperature to obtain the polyethyleneimine modified AKD;
s4, weighing 200 parts of AKD modified by polyethyleneimine in S3 and a proper amount of deionized water, adding into a three-neck flask, stirring, heating at 60 ℃ until the AKD is completely melted, adding 8 parts of titanium dioxide modified by dopamine in S1 and 20 parts of mixed emulsifier in S2 after increasing the rotating speed, premixing for 5min, and transferring into a homogenizer;
s5, adding a dispersing agent and a synergistic agent into the system of the homogenizer in S4, uniformly mixing, shearing and emulsifying for 15min at a high speed of 10000r/min by using a high-shearing emulsifying machine, cooling to room temperature, adding 14 parts of polyaluminium chloride, and uniformly mixing to obtain the AKD emulsion.
In S1, the mass ratio of dopamine to titanium dioxide is 3:2.
the stirring speed in S1 was 500r/min.
The preparation method of the composite cationic starch emulsifier in S2 comprises the following steps:
step 1: adding 50 parts of corn starch, 2 parts of ammonium persulfate, 1 part of cross-linking agent and 3 parts of high-positive-charge acrylic ester polymer into a flask, and gelatinizing for 30min at 95 ℃;
step 2: adding a proper amount of deionized water into the system in the step 1 for dilution, and then adjusting the pH value to 3 by using acetic acid to obtain the composite cationic starch emulsifier.
The preparation method of the compound emulsifier in S2 comprises the following steps:
step one: weighing 2 parts of nonionic surfactant and 1 part of cationic surfactant, pouring into a beaker, adding a proper amount of solvent, and mixing and stirring;
step two: and (3) uniformly stirring the system in the step one, and then performing ultrasonic dispersion for 15min at the frequency of 12000Hz to obtain the compound emulsifier.
The water bath temperature in S3 was 70 ℃.
The stirring speed in S4 was 400r/min.
The dispersant in S5 is hexenyl bis stearamide.
The synergist in S5 is modified guar gum powder.
The preparation method of the modified guar gum comprises the following steps: adding alkali liquor into a reaction kettle, adding guar gum powder under the stirring condition of 400rpm, adding galactose oxidase and mannase when the stirring speed is increased to 600rpm, uniformly dispersing, reacting for 3 hours at 130 ℃, pouring the obtained product into an ethanol water solution, regulating the pH value to 7, filtering out supernatant, washing the precipitate by using the ethanol water solution, and drying and crushing to obtain modified guar gum powder.
Performance testing
The AKD emulsions based on the dopamine-modified titanium dioxide obtained in examples 1 to 3 were marked as example 1, example 2 and example 3, respectively, and the AKD emulsions which are common in the market were marked as comparative examples, and the properties thereof were measured, respectively, and the measurement results were recorded in the following table:
as shown by the data in the table, the performance of the AKD emulsion based on the dopamine-modified titanium dioxide in the embodiment 1-3 is obviously higher than that of the common AKD emulsion on the market, and the AKD emulsion based on the dopamine-modified titanium dioxide has excellent stability and adhesive viscosity, so that the AKD based on the dopamine-modified titanium dioxide prepared by the invention has excellent market popularization value.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. An AKD production process based on dopamine modified titanium dioxide is characterized by comprising the following production steps:
s1, weighing 40 parts of sodium hydroxide, placing the sodium hydroxide into a beaker, adding 1000ml of deionized water, uniformly stirring, heating to 35-40 ℃, weighing a proper amount of dopamine, adding the dopamine into the beaker, stirring, weighing a proper amount of titanium dioxide, adding the titanium dioxide into the beaker, reacting for a period of time under the condition of keeping the temperature unchanged, finally carrying out suction filtration on the product, washing the product for a plurality of times by using the deionized water, placing the washed product into a 60 ℃ oven for drying, and grinding the dried product to obtain the dopamine-modified titanium dioxide;
s2, according to 10:1, mixing the composite cationic starch emulsifier and the compound emulsifier in a mass ratio, and uniformly mixing to obtain a mixed emulsifier;
s3, heating and melting AKD wax powder in a water bath, slowly adding the preheated polyethyleneimine solution into the melted AKD after the AKD is completely melted, adding a proper amount of deionized water after high-speed shearing and stirring for 1min, continuing high-speed shearing and stirring for 10min, standing for 1h, and cooling to normal temperature to obtain the polyethyleneimine modified AKD;
s4, weighing 200 parts of AKD modified by polyethyleneimine in S3 and a proper amount of deionized water, adding into a three-neck flask, stirring, heating at 60 ℃ until the AKD is completely melted, adding 8-10 parts of titanium dioxide modified by dopamine in S1 and 16-20 parts of mixed emulsifier in S2 after increasing the rotating speed, premixing for 5min, and transferring into a homogenizer;
s5, adding a dispersing agent and a synergistic agent into the system of the homogenizer in S4, uniformly mixing, shearing and emulsifying for 10-20min at a high speed of 10000r/min by using a high-shearing emulsifying machine, cooling to room temperature, adding 13-15 parts of polyaluminium chloride, and uniformly mixing to obtain AKD emulsion;
the preparation method of the composite cationic starch emulsifier in the step S2 comprises the following steps:
step 1: adding 50 parts of corn starch, 1-2 parts of ammonium persulfate, 1-2 parts of cross-linking agent and 3-4 parts of high-positive-charge acrylic ester polymer into a flask, and gelatinizing for 30min at 95 ℃;
step 2: adding a proper amount of deionized water into the system in the step 1 for dilution, and then adjusting the pH value to 3 by using acetic acid to obtain the composite cationic starch emulsifier;
the preparation method of the compound emulsifier in the S2 comprises the following steps:
step one: weighing 2 parts of nonionic surfactant and 1 part of cationic surfactant, pouring into a beaker, adding a proper amount of solvent, and mixing and stirring;
step two: and (3) uniformly stirring the system in the step one, and then performing ultrasonic dispersion for 15min at the frequency of 10000-12000Hz to obtain the compound emulsifier.
2. The AKD manufacturing process based on dopamine-modified titanium dioxide according to claim 1, wherein the mass ratio of dopamine to titanium dioxide in S1 is 3:2.
3. the AKD production process based on dopamine-modified titanium dioxide according to claim 1, wherein the stirring speed in S1 is 500r/min.
4. The AKD production process based on dopamine-modified titanium dioxide according to claim 1, characterized in that the water bath temperature in S3 is 70-80 ℃.
5. The AKD production process based on dopamine-modified titanium dioxide according to claim 1, wherein the stirring speed in S4 is 300-500r/min.
6. The AKD production process based on dopamine-modified titanium dioxide according to claim 1, wherein the dispersant in S5 is hexenyl bis stearamide.
7. The AKD production process based on dopamine-modified titanium dioxide according to claim 1, wherein the synergist in S5 is modified guar gum powder.
8. The AKD manufacturing process based on dopamine-modified titanium dioxide according to claim 7, characterized in that the modified guar gum powder is prepared by the following method: adding alkali liquor into a reaction kettle, adding guar gum powder under the stirring condition of 300-400rpm, adding galactose oxidase and mannase when the stirring speed is increased to 600-800rpm, uniformly dispersing, reacting for 3-4 hours at 120-130 ℃, pouring the obtained product into an ethanol water solution to adjust the pH value to 7, filtering out supernatant, washing the precipitate by using the ethanol water solution, and drying and crushing to obtain the modified guar gum powder.
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| CN101748658A (en) * | 2009-12-09 | 2010-06-23 | 青岛科技大学 | Preparation of polyethyleneimine AKD new type sizing agent |
| CN101949108B (en) * | 2010-10-29 | 2013-04-24 | 天津市奥东化工有限公司 | Polyethyleneimine-modified AKD sizing agent and preparation method thereof |
| CN102614783B (en) * | 2012-03-27 | 2013-12-25 | 大连理工大学 | Method for preparing high-flux composite membrane from dopamine-modified nanometer material |
| CN102627734B (en) * | 2012-05-04 | 2013-06-05 | 陕西科技大学 | Preparation method of amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent without sizing lag |
| CN102635033B (en) * | 2012-05-04 | 2014-05-14 | 陕西科技大学 | Preparation method of no-sizing lag beewax/AKD (alkyl ketene dimer) neutral/alkaline sizing agent |
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