CN108676347A - A kind of preparation method of the special antistatic agent of polyurethane plastics - Google Patents
A kind of preparation method of the special antistatic agent of polyurethane plastics Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the special antistatic agent of polyurethane plastics, belong to technical field of polymer materials.By pre- modified alta-mud and water in mass ratio 1：10~1：15 mixing adjust pH to 10.0~10.5, and the modifying agent of 0.1~0.3 times of pre- modified alta-mud quality are added, and after being stirred, filtering pulverizes and sieves, obtains modified alta-mud；By pre- modified glass-fiber and water in mass ratio 1：5~1：10 mixing, and the silane coupling agent of 1~2 times of pre- modified glass-fiber quality is added, after being stirred, filter, it is dry, obtain modified glass-fiber；By modified alta-mud and modified glass-fiber in mass ratio 3：1~4：1 mixing is to get the special antistatic agent of polyurethane plastics.The gained special antistatic agent of polyurethane plastics of the invention has excellent antistatic effect.
Description
Technical field
The invention discloses a kind of preparation methods of the special antistatic agent of polyurethane plastics, belong to high polymer material technology neck
Domain.
Background technology
Along with the development of science and technology, the application of high molecular material is increasingly extensive.However, high molecular material has high surface
Resistance and volume resistance, once be charged by friction, electrostatic not easily passs through conductive remove and is trapped in material surface, can not only influence
Appearance characteristics, manufacture and the use of material are especially made in coal Deng Kuang factories underground more important is there are electrostatic safety hidden danger
In the environment of industry, the use of high molecular material must carry out antistatic surface processing.In order to eliminate electrostatic, usually in macromolecule material
Corresponding antistatic agent is added in material, to reduce sheet resistance and volume resistance, expands its use scope.Weigh macromolecule material
Material antistatic property quality refers mainly to indicate：Sheet resistance, electrostatic half-life, hygroscopicity（Contact angle）, saturation electrostatic potential
Deng dividing the grade of high molecular material antistatic property according to charge half life and sheet resistance.
The type of antistatic agent is various, and currently used mainly surfactant can be divided into cation by chemical constitution
Type, anionic, nonionic, amphoteric, polymer electrolyte, different types of antistatic agent have different structures, using model
It encloses and respective advantage and disadvantage.In addition, composite antistatic agent has been to be concerned by more and more people and favors.It is compound antistatic
Agent is the new varieties of antistatic agent, it is developed using the synergistic effect principle between each component.Because of single use
Often there is certain defect in certain antistatic agent, ideal effect is extremely difficult in certain antistatic more demanding places,
Derivative of fatty acid such as hydroxyethylation amine, polyol esters of fatty acids and alkanolamide is compound, and being applied to polyethylene, polypropylene can
Obtain apparent antistatic effect.There is also the bad problems of antistatic effect for traditional antistatic agent at present, therefore also need pair
It is studied.
Invention content
The present invention solves the technical problem of：For the bad problem of conventional antistatic agents antistatic effect, provide
A kind of preparation method of the special antistatic agent of polyurethane plastics.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Sodium bentonite is crushed and is sieved, refinement sodium bentonite is obtained, by refinement sodium bentonite and water in mass ratio 1：40
~1：50 mixing, and the green vitriol of 4~5 times of refinement sodium bentonite quality is added, under nitrogen protection, after being aerated 5~10min,
Bentonite mixtures must be pre-processed, by pretreatment bentonite mixtures and no oxyethanol in mass ratio 3：1~4：1 mixing, obtains swollen
Moisten earth mixtures；
（2）By potassium borohydride and sodium hydroxide solution in mass ratio 1：10~1：15 mixing, obtain sodium hydroxide mixed liquor, by swelling
The sodium hydroxide mixed liquor of 0.2~0.4 times of earth mixtures quality instills in bentonite mixtures, and after being stirred, filtering must filter
Filter cake anaerobic milli-Q water is used in combination deoxidation absolute ethyl alcohol to wash by cake, dry, obtains pre- modified alta-mud；
（3）By pre- modified alta-mud and water in mass ratio 1：10~1：15 mixing adjust pH to 10.0~10.5, and are added and change in advance
Property 0.1~0.3 times of bentonite quality modifying agent, after being stirred, filtering pulverizes and sieves, obtains modified alta-mud；
（4）By glass fibre and inorganic agent in mass ratio 1：5~1：8 mixing are impregnated, and filtering obtains pretreated glass fiber, will be pre-
Handle glass fibre and graphene oxide liquid mixture in mass ratio 1：10~1：20 mixing, impregnate, and filter, dry, obtain 1 processing
Glass fibre, by 1 processing glass fibre and chitosan solution in mass ratio 1：10~1：15 mixing, impregnate, and filter, dry,
Obtain pre- modified glass-fiber；
（5）By pre- modified glass-fiber and water in mass ratio 1：5~1：10 mixing, and pre- modified glass-fiber quality 1~2 is added
Silane coupling agent again after being stirred, filters, dry, obtains modified glass-fiber；
（6）By modified alta-mud and modified glass-fiber in mass ratio 3：1~4：1 mixing is special anti-quiet to get polyurethane plastics
Electric agent.
Step（3）The modifying agent is any one in cetyl trimethylammonium bromide or N- Alkylation of Amino Acids.
Step（4）The length of the glass fibre is 1~2mm, a diameter of 0.1~0.3mm.
Step（4）The inorganic agent be 60~70% by mass fraction sulfuric acid and hydrogen peroxide by volume 3：1 is mixed
It closes, obtains inorganic agent.
Step（4）The preparation method of the graphene oxide liquid mixture is by graphene oxide and water in mass ratio 1：100
~1：300 mixing, ultrasonic disperse are used in combination sodium hydroxide to adjust pH to 7.0~7.2, obtain graphene oxide liquid mixture.
Step（4）The preparation method of the chitosan solution is by chitosan and water in mass ratio 1：200~1：300 is mixed
It closes, is used in combination second acid for adjusting pH to 4.0~4.2, obtains chitosan solution.
Step（5）The silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent
Any one in KH-570.
The beneficial effects of the invention are as follows：
（1）Modified alta-mud is added when preparing the special antistatic agent of polyurethane plastics in the present invention, and bentonite is modified first
Before first pass through pre- modification, so that bentonite surface is fixed with fe, after being added in product, due to the presence of iron, to
Make the high molecular material of addition product that there is preferable electric conductivity, secondly, pre- modified alta-mud is after modification, swelling
Soil is changed into lipophile by hydrophily, to which after being added in high molecular material, modified alta-mud can be dispersed in macromolecule
In material, and since the fe sodium metasilicate being added in the process that can be modified that modified alta-mud surface carries is coated, from
And after modified alta-mud is added in high molecular material, fe can be together scattered in bentonite in high molecular material, to
Make product that can effectively improve the antistatic effect of high molecular material；
（2）Modified glass-fiber is added when preparing the special antistatic agent of polyurethane plastics in the present invention, on the one hand, glass fibre exists
After modification, fiberglass surfacing is covered by graphene oxide and chitosan, to make the electric conductivity of glass fibre carry
Height, and then the antistatic effect of product is made to improve, on the other hand, silane coupling agent is added to glass in glass fibre in modifying process
Glass fiber is handled, can be with modification to make glass fibre that can be uniformly distributed in high molecular material after being added in product
Bentonite forms good conductive path inside high molecular material, and then the antistatic effect of product is made to further increase, and
And since modified alta-mud and modified glass-fiber are dispersed in high molecular material, so as to make high molecular material that there is length
The antistatic property of effect.
Specific implementation mode
Sodium bentonite was crushed into 180 mesh sieve, obtains refinement sodium bentonite, refinement sodium bentonite and water are pressed into quality
Than 1：40~1：50 are mixed in three-necked flask, are 30~40 DEG C in temperature, under conditions of rotating speed is 200~300r/min, stir
After mixing 22~26h of mixing, the green vitriol of 4~5 times of refinement sodium bentonite quality is added into three-necked flask, and into three-necked flask
It is passed through nitrogen with the rate of 15~20mL/min, after being aerated 5~10min under nitrogen atmosphere, obtains pretreatment bentonite mixtures,
It will pretreatment bentonite mixtures and no oxyethanol in mass ratio 3：1~4：1 mixing, in temperature be 25~35 DEG C, rotating speed 220
Under conditions of~350r/min, after being stirred 20~40min, bentonite mixtures are obtained；By potassium borohydride and mass fraction 0.1
~0.2% sodium hydroxide solution in mass ratio 1：8~1：15 mixing are 30~45 DEG C in temperature, and rotating speed is 200~350r/
The condition of min after being stirred 20~30min, obtains sodium hydroxide mixed liquor, by 0.2~0.5 times of bentonite mixtures quality
Sodium hydroxide mixed liquor is instilled with the rate of 2~7mL/min in bentonite mixtures, and is 30~40 DEG C in temperature, and rotating speed is
It is stirred under conditions of 500~800r/min to sodium hydroxide mixing drop and is use up, it is 30~40 DEG C to continue at temperature, and rotating speed is
After the condition of 500~800r/min is stirred 30~40min, filtering obtains filter cake, by filter cake anaerobic milli-Q water 3~8
It is secondary, after being used in combination deoxidation absolute ethyl alcohol to wash 5~8 times, dry 15 under conditions of being 60~70 DEG C in temperature by the filter cake after washing
~40min obtains pre- modified alta-mud, by pre- modified alta-mud and water in mass ratio 1：10~1：15 are mixed in beaker, use silicon
Sour sodium adjusts the pH of material in beaker to 10.0~10.5, and 0.1~0.3 times of pre- modified alta-mud quality is added into beaker
Modifying agent is 40~55 DEG C in temperature, and after rotating speed is stirred 1~2h under conditions of being 300~350r/min, filtering must change
Property bentonite blank, by modified alta-mud blank crushed 220 mesh sieve, obtain modified alta-mud；Glass fibre and inorganic agent are pressed
Mass ratio 1：5~1：8 mixing, and after impregnating 40~50min under room temperature, filtering obtains pretreated glass fiber, will locate in advance
Manage glass fibre and graphene oxide liquid mixture in mass ratio 1：10~1：20 mixing are soaked under conditions of being 40~50 DEG C in temperature
Steep 15~30min after, filtering, must pre-process 1 time processing glass fibre, will pretreatment 1 time processing glass fibre in temperature be 50
Under conditions of~70 DEG C after dry 30~40min, 1 processing glass fibre is obtained, by 1 processing glass fibre and chitosan solution
In mass ratio 1：10~1：15 mixing, after impregnating 15~30min under conditions of being 40~50 DEG C in temperature, filtering obtains pre- modification
Glass fibre blank obtains pre- under conditions of being 60~80 DEG C in temperature by pre- modified glass-fiber blank after dry 20~30min
Modified glass-fiber；By pre- modified glass-fiber and water in mass ratio 1：5~1：10 mixing, and to pre- modified glass-fiber and water
Mixture in the silane coupling agent of 1~2 times of pre- modified glass-fiber quality is added, in temperature be 45~55 DEG C, rotating speed 200
After being stirred 2~3h under conditions of~300r/min, filtering obtains pretreatment modification glass fibre, by pretreatment modification glass
Under conditions of fiber is 60~80 DEG C in temperature after dry 30~40min, modified glass-fiber is obtained；By modified alta-mud and modification
Glass fibre in mass ratio 3：1~4：1 is mixed in blender, is 40~50 DEG C in temperature, rotating speed is 300~450r/min's
Under the conditions of, it is stirred after 40~50min to get the special antistatic agent of polyurethane plastics.The modifying agent is cetyl three
Any one in methyl bromide ammonium or N- Alkylation of Amino Acids.The length of the glass fibre be 1~2mm, a diameter of 0.1~
0.3mm.The inorganic agent be 60~70% by mass fraction sulfuric acid and hydrogen peroxide by volume 3：1 mixing, must be handled
Agent.The preparation method of the graphene oxide liquid mixture is by graphene oxide and water in mass ratio 1：100~1：300 mixing,
Ultrasonic disperse is used in combination sodium hydroxide to adjust pH to 7.0~7.2, obtains graphene oxide liquid mixture.The preparation of the chitosan solution
Method is by chitosan and water in mass ratio 1：200~1：300 mixing, are used in combination second acid for adjusting pH to 4.0~4.2, obtain chitosan
Solution.The silane coupling agent is silane resin acceptor kh-550, is appointed in silane coupling agent KH-560 or Silane coupling reagent KH-570
Meaning is a kind of.
Sodium bentonite was crushed into 180 mesh sieve, obtains refinement sodium bentonite, refinement sodium bentonite and water are pressed into quality
Than 1：50 are mixed in three-necked flask, in temperature be 40 DEG C, rotating speed be 300r/min under conditions of, after being stirred 26h, to three
The green vitriol of 5 times of refinement sodium bentonite quality is added in mouth flask, and nitrogen is passed through with the rate of 20mL/min into three-necked flask
Gas obtains pretreatment bentonite mixtures after being aerated 10min under nitrogen atmosphere, by pretreatment bentonite mixtures and anaerobic second
Alcohol in mass ratio 4：1 mixing is 35 DEG C in temperature, under conditions of rotating speed is 350r/min, after being stirred 40min, obtains swelling
Earth mixtures；By the sodium hydroxide solution in mass ratio 1 of potassium borohydride and mass fraction 0.2%：15 mixing, in temperature be 45 DEG C,
Rotating speed is the condition of 350r/min, after being stirred 30min, obtains sodium hydroxide mixed liquor, by 0.5 times of bentonite mixtures quality
Sodium hydroxide mixed liquor instilled in bentonite mixtures with the rate of 7mL/min, and in temperature be 40 DEG C, rotating speed 800r/
It is stirred under conditions of min to sodium hydroxide mixing drop and is use up, it is 40 DEG C to continue at temperature, and rotating speed is the condition of 800r/min
After being stirred 40min, filtering obtains filter cake, and by filter cake anaerobic milli-Q water 8 times, deoxidation absolute ethyl alcohol washing 8 times be used in combination
Afterwards, by the filter cake after washing be 70 DEG C in temperature under conditions of dry 40min, pre- modified alta-mud is obtained, by pre- modified alta-mud
With water in mass ratio 1：15 are mixed in beaker, with the pH of material in sodium metasilicate adjusting beaker to 10.5, and are added into beaker
The modifying agent of 0.3 times of pre- modified alta-mud quality is 55 DEG C in temperature, and rotating speed is stirred 2h under conditions of being 350r/min
Afterwards, it filters, obtains modified alta-mud blank, modified alta-mud blank be crushed into 220 mesh sieve, obtain modified alta-mud；By glass fibers
Dimension and inorganic agent in mass ratio 1：8 mixing, and after impregnating 50min under room temperature, filtering obtains pretreated glass fiber, it will
Pretreated glass fiber and graphene oxide liquid mixture in mass ratio 1：20 mixing are impregnated under conditions of being 50 DEG C in temperature
After 30min, filtering must pre-process 1 processing glass fibre, the item for being 70 DEG C in temperature by 1 processing glass fibre of pretreatment
Under part after dry 40min, 1 processing glass fibre is obtained, by 1 processing glass fibre and chitosan solution in mass ratio 1：15 is mixed
It closes, after impregnating 30min under conditions of being 50 DEG C in temperature, filtering obtains pre- modified glass-fiber blank, by pre- modified glass-fiber
Under conditions of blank is 80 DEG C in temperature after dry 30min, pre- modified glass-fiber is obtained；Pre- modified glass-fiber and water are pressed into matter
Measure ratio 1：10 mix, and the silane of pre- 2 times of modified glass-fiber quality is added into the mixture of pre- modified glass-fiber and water
Coupling agent is 55 DEG C in temperature, and after rotating speed is stirred 3h under conditions of being 300r/min, filtering obtains pretreatment modification glass
Fiber obtains modified glass-fiber under conditions of being 80 DEG C in temperature by pretreatment modification glass fibre after dry 40min；It will change
Property bentonite and modified glass-fiber in mass ratio 4：1 is mixed in blender, is 50 DEG C in temperature, rotating speed is 450r/min's
Under the conditions of, it is stirred after 50min to get the special antistatic agent of polyurethane plastics.The modifying agent is cetyl trimethyl
Ammonium bromide.The length of the glass fibre is 2mm, a diameter of 0.3mm.The inorganic agent be 70% by mass fraction sulfuric acid
With hydrogen peroxide by volume 3：1 mixing, obtains inorganic agent.The preparation method of the graphene oxide liquid mixture is by graphite oxide
Alkene and water in mass ratio 1：300 mixing, ultrasonic disperse are used in combination sodium hydroxide to adjust pH to 7.2, obtain graphene oxide liquid mixture.
The preparation method of the chitosan solution is by chitosan and water in mass ratio 1：300 mixing, are used in combination second acid for adjusting pH to 4.2,
Obtain chitosan solution.The silane coupling agent is silane resin acceptor kh-550.
Sodium bentonite was crushed into 180 mesh sieve, obtains refinement sodium bentonite, refinement sodium bentonite and water are pressed into quality
Than 1：50 are mixed in three-necked flask, in temperature be 40 DEG C, rotating speed be 300r/min under conditions of, after being stirred 26h, to three
The green vitriol of 5 times of refinement sodium bentonite quality is added in mouth flask, and nitrogen is passed through with the rate of 20mL/min into three-necked flask
Gas obtains pretreatment bentonite mixtures after being aerated 10min under nitrogen atmosphere, by pretreatment bentonite mixtures and anaerobic second
Alcohol in mass ratio 4：1 mixing is 35 DEG C in temperature, under conditions of rotating speed is 350r/min, after being stirred 40min, obtains swelling
Earth mixtures；By bentonite mixtures and water in mass ratio 1：15 are mixed in beaker, and material in beaker is adjusted with sodium metasilicate
The modifying agent of 0.3 times of bentonite mixtures quality is added into beaker to 10.5 in pH, in temperature be 55 DEG C, rotating speed 350r/
After being stirred 2h under conditions of min, filtering obtains modified alta-mud blank, and modified alta-mud blank crushed 220 mesh sieve,
Obtain modified alta-mud；By glass fibre and inorganic agent in mass ratio 1：8 mixing, and after impregnating 50min under room temperature, mistake
Filter, obtains pretreated glass fiber, by pretreated glass fiber and graphene oxide liquid mixture in mass ratio 1：20 mixing, in temperature
After impregnating 30min under conditions of being 50 DEG C, filtering must pre-process 1 processing glass fibre, by 1 processing glass fibers of pretreatment
Tie up be 70 DEG C in temperature under conditions of after dry 40min, 1 processing glass fibre is obtained, by 1 processing glass fibre and chitosan
Solution in mass ratio 1：15 mixing, after impregnating 30min under conditions of being 50 DEG C in temperature, filtering obtains pre- modified glass-fiber base
Material obtains pre- modified glass-fiber under conditions of being 80 DEG C in temperature by pre- modified glass-fiber blank after dry 30min；It will be pre-
Modified glass-fiber and water in mass ratio 1：10 mixing, and pre- modified glass is added into the mixture of pre- modified glass-fiber and water
The silane coupling agent that 2 times of glass fiber quality, in temperature be 55 DEG C, rotating speed be 300r/min under conditions of be stirred 3h after, mistake
Filter, obtains pretreatment modification glass fibre, under conditions of being 80 DEG C in temperature by pretreatment modification glass fibre after dry 40min,
Obtain modified glass-fiber；By modified alta-mud and modified glass-fiber in mass ratio 4：1 is mixed in blender, in temperature be 50
DEG C, under conditions of rotating speed is 450r/min, it is stirred after 50min to get the special antistatic agent of polyurethane plastics.The modification
Agent is cetyl trimethylammonium bromide.The length of the glass fibre is 2mm, a diameter of 0.3mm.The inorganic agent is by matter
Measure sulfuric acid and hydrogen peroxide that score is 70% by volume 3：1 mixing, obtains inorganic agent.The system of the graphene oxide liquid mixture
Preparation Method is by graphene oxide and water in mass ratio 1：300 mixing, ultrasonic disperse are used in combination sodium hydroxide to adjust pH to 7.2, are obtained
Graphene oxide liquid mixture.The preparation method of the chitosan solution is by chitosan and water in mass ratio 1：300 mixing, are used in combination
Second acid for adjusting pH obtains chitosan solution to 4.2.The silane coupling agent is silane resin acceptor kh-550.
Sodium bentonite was crushed into 180 mesh sieve, obtains refinement sodium bentonite, refinement sodium bentonite and water are pressed into quality
Than 1：50 are mixed in three-necked flask, in temperature be 40 DEG C, rotating speed be 300r/min under conditions of, after being stirred 26h, to three
The green vitriol of 5 times of refinement sodium bentonite quality is added in mouth flask, and nitrogen is passed through with the rate of 20mL/min into three-necked flask
Gas obtains pretreatment bentonite mixtures after being aerated 10min under nitrogen atmosphere, by pretreatment bentonite mixtures and anaerobic second
Alcohol in mass ratio 4：1 mixing is 35 DEG C in temperature, under conditions of rotating speed is 350r/min, after being stirred 40min, obtains swelling
Earth mixtures；By the sodium hydroxide solution in mass ratio 1 of potassium borohydride and mass fraction 0.2%：15 mixing, in temperature be 45 DEG C,
Rotating speed is the condition of 350r/min, after being stirred 30min, obtains sodium hydroxide mixed liquor, by 0.5 times of bentonite mixtures quality
Sodium hydroxide mixed liquor instilled in bentonite mixtures with the rate of 7mL/min, and in temperature be 40 DEG C, rotating speed 800r/
It is stirred under conditions of min to sodium hydroxide mixing drop and is use up, it is 40 DEG C to continue at temperature, and rotating speed is the condition of 800r/min
After being stirred 40min, filtering obtains filter cake, and by filter cake anaerobic milli-Q water 8 times, deoxidation absolute ethyl alcohol washing 8 times be used in combination
Afterwards, by the filter cake after washing be 70 DEG C in temperature under conditions of dry 40min, obtain pre- modified alta-mud；By glass fibre and place
Manage agent in mass ratio 1：8 mixing, and after impregnating 50min under room temperature, filtering obtains pretreated glass fiber, will pre-process
Glass fibre and graphene oxide liquid mixture in mass ratio 1：20 mixing, after impregnating 30min under conditions of being 50 DEG C in temperature, mistake
Filter must pre-process 1 processing glass fibre, dry under conditions of being 70 DEG C in temperature by 1 processing glass fibre of pretreatment
After 40min, 1 processing glass fibre is obtained, by 1 processing glass fibre and chitosan solution in mass ratio 1：15 mixing, Yu Wen
After degree is impregnates 30min under conditions of 50 DEG C, filtering obtains pre- modified glass-fiber blank, by pre- modified glass-fiber blank in
Temperature after dry 30min, obtains pre- modified glass-fiber under conditions of being 80 DEG C；By pre- modified glass-fiber and water in mass ratio 1：
10 mix, and the silane coupling agent of pre- 2 times of modified glass-fiber quality is added into the mixture of pre- modified glass-fiber and water,
It it is 55 DEG C in temperature, after rotating speed is stirred 3h under conditions of being 300r/min, filtering obtains pretreatment modification glass fibre, will
Under conditions of pretreatment modification glass fibre is 80 DEG C in temperature after dry 40min, modified glass-fiber is obtained；By pre- bentone
Soil and modified glass-fiber in mass ratio 4：1 is mixed in blender, is 50 DEG C in temperature, rotating speed is the condition of 450r/min
Under, it is stirred after 50min to get the special antistatic agent of polyurethane plastics.The modifying agent is cetyl trimethyl bromination
Ammonium.The length of the glass fibre is 2mm, a diameter of 0.3mm.The inorganic agent be by mass fraction be 70% sulfuric acid and mistake
Hydrogen oxide by volume 3：1 mixing, obtains inorganic agent.The preparation method of the graphene oxide liquid mixture be by graphene oxide with
Water in mass ratio 1：300 mixing, ultrasonic disperse are used in combination sodium hydroxide to adjust pH to 7.2, obtain graphene oxide liquid mixture.It is described
The preparation method of chitosan solution is by chitosan and water in mass ratio 1：300 mixing, are used in combination second acid for adjusting pH to 4.2, obtain shell
Glycan solution.The silane coupling agent is silane resin acceptor kh-550.
Sodium bentonite was crushed into 180 mesh sieve, obtains refinement sodium bentonite, refinement sodium bentonite and water are pressed into quality
Than 1：50 are mixed in three-necked flask, in temperature be 40 DEG C, rotating speed be 300r/min under conditions of, after being stirred 26h, to three
The green vitriol of 5 times of refinement sodium bentonite quality is added in mouth flask, and nitrogen is passed through with the rate of 20mL/min into three-necked flask
Gas obtains pretreatment bentonite mixtures after being aerated 10min under nitrogen atmosphere, by pretreatment bentonite mixtures and anaerobic second
Alcohol in mass ratio 4：1 mixing is 35 DEG C in temperature, under conditions of rotating speed is 350r/min, after being stirred 40min, obtains swelling
Earth mixtures；By the sodium hydroxide solution in mass ratio 1 of potassium borohydride and mass fraction 0.2%：15 mixing, in temperature be 45 DEG C,
Rotating speed is the condition of 350r/min, after being stirred 30min, obtains sodium hydroxide mixed liquor, by 0.5 times of bentonite mixtures quality
Sodium hydroxide mixed liquor instilled in bentonite mixtures with the rate of 7mL/min, and in temperature be 40 DEG C, rotating speed 800r/
It is stirred under conditions of min to sodium hydroxide mixing drop and is use up, it is 40 DEG C to continue at temperature, and rotating speed is the condition of 800r/min
After being stirred 40min, filtering obtains filter cake, and by filter cake anaerobic milli-Q water 8 times, deoxidation absolute ethyl alcohol washing 8 times be used in combination
Afterwards, by the filter cake after washing be 70 DEG C in temperature under conditions of dry 40min, pre- modified alta-mud is obtained, by pre- modified alta-mud
With water in mass ratio 1：15 are mixed in beaker, with the pH of material in sodium metasilicate adjusting beaker to 10.5, and are added into beaker
The modifying agent of 0.3 times of pre- modified alta-mud quality is 55 DEG C in temperature, and rotating speed is stirred 2h under conditions of being 350r/min
Afterwards, it filters, obtains modified alta-mud blank, modified alta-mud blank be crushed into 220 mesh sieve, obtain modified alta-mud；By glass fibers
Dimension and water in mass ratio 1：10 mixing, and the silane of 2 times of glass fiber quality of addition is even into the mixture of glass fibre and water
Join agent, is 55 DEG C in temperature, after rotating speed is stirred 3h under conditions of being 300r/min, filtering obtains pretreatment modification glass fibers
Dimension obtains modified glass-fiber under conditions of being 80 DEG C in temperature by pretreatment modification glass fibre after dry 40min；It will be modified
Bentonite and modified glass-fiber in mass ratio 4：1 is mixed in blender, is 50 DEG C in temperature, rotating speed is the item of 450r/min
Under part, it is stirred after 50min to get the special antistatic agent of polyurethane plastics.The modifying agent is cetyl trimethyl bromine
Change ammonium.The length of the glass fibre is 2mm, a diameter of 0.3mm.The inorganic agent be by mass fraction be 70% sulfuric acid with
Hydrogen peroxide by volume 3：1 mixing, obtains inorganic agent.The preparation method of the graphene oxide liquid mixture is by graphene oxide
With water in mass ratio 1：300 mixing, ultrasonic disperse are used in combination sodium hydroxide to adjust pH to 7.2, obtain graphene oxide liquid mixture.Institute
The preparation method for stating chitosan solution is by chitosan and water in mass ratio 1：300 mixing, are used in combination second acid for adjusting pH to 4.2, obtain
Chitosan solution.The silane coupling agent is silane resin acceptor kh-550.
Comparative example：The antistatic agent of Shanghai Chemical Co., Ltd. production.
1 to 4 gained antistatic agent of example and comparative example product are subjected to performance detection, specific detection method is as follows：
Above-mentioned antistatic agent is added in polyurethane plastics, detects its surface resistivity, specific testing result is as shown in table 1：
Table 1：Performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Surface resistivity/Ω | 3.2×107 | 8.48×108 | 3.45×109 | 1.82×109 | 5.0×1010 |
By 1 testing result of table it is found that the present invention gained special antistatic agent of polyurethane plastics has excellent antistatic effect.
Claims (7)
1. a kind of preparation method of the special antistatic agent of polyurethane plastics, which is characterized in that specifically preparation process is：
（1）Sodium bentonite is crushed and is sieved, refinement sodium bentonite is obtained, by refinement sodium bentonite and water in mass ratio 1：40
~1：50 mixing, and the green vitriol of 4~5 times of refinement sodium bentonite quality is added, under nitrogen protection, after being aerated 5~10min,
Bentonite mixtures must be pre-processed, by pretreatment bentonite mixtures and no oxyethanol in mass ratio 3：1~4：1 mixing, obtains swollen
Moisten earth mixtures；
（2）By potassium borohydride and sodium hydroxide solution in mass ratio 1：10~1：15 mixing, obtain sodium hydroxide mixed liquor, by swelling
The sodium hydroxide mixed liquor of 0.2~0.4 times of earth mixtures quality instills in bentonite mixtures, and after being stirred, filtering must filter
Filter cake anaerobic milli-Q water is used in combination deoxidation absolute ethyl alcohol to wash by cake, dry, obtains pre- modified alta-mud；
（3）By pre- modified alta-mud and water in mass ratio 1：10~1：15 mixing adjust pH to 10.0~10.5, and are added and change in advance
Property 0.1~0.3 times of bentonite quality modifying agent, after being stirred, filtering pulverizes and sieves, obtains modified alta-mud；
（4）By glass fibre and inorganic agent in mass ratio 1：5~1：8 mixing are impregnated, and filtering obtains pretreated glass fiber, will be pre-
Handle glass fibre and graphene oxide liquid mixture in mass ratio 1：10~1：20 mixing, impregnate, and filter, dry, obtain 1 processing
Glass fibre, by 1 processing glass fibre and chitosan solution in mass ratio 1：10~1：15 mixing, impregnate, and filter, dry,
Obtain pre- modified glass-fiber；
（5）By pre- modified glass-fiber and water in mass ratio 1：5~1：10 mixing, and pre- modified glass-fiber quality 1~2 is added
Silane coupling agent again after being stirred, filters, dry, obtains modified glass-fiber；
（6）By modified alta-mud and modified glass-fiber in mass ratio 3：1~4：1 mixing is special anti-quiet to get polyurethane plastics
Electric agent.
2. a kind of preparation method of the special antistatic agent of polyurethane plastics according to claim 1, it is characterised in that：Step
（3）The modifying agent is any one in cetyl trimethylammonium bromide or N- Alkylation of Amino Acids.
3. a kind of preparation method of the special antistatic agent of polyurethane plastics according to claim 1, it is characterised in that：Step
（4）The length of the glass fibre is 1~2mm, a diameter of 0.1~0.3mm.
4. a kind of preparation method of the special antistatic agent of polyurethane plastics according to claim 1, it is characterised in that：Step
（4）The inorganic agent be 60~70% by mass fraction sulfuric acid and hydrogen peroxide by volume 3：1 mixing, obtains inorganic agent.
5. a kind of preparation method of the special antistatic agent of polyurethane plastics according to claim 1, it is characterised in that：Step
（4）The preparation method of the graphene oxide liquid mixture is by graphene oxide and water in mass ratio 1：100~1：300 mixing,
Ultrasonic disperse is used in combination sodium hydroxide to adjust pH to 7.0~7.2, obtains graphene oxide liquid mixture.
6. a kind of preparation method of the special antistatic agent of polyurethane plastics according to claim 1, it is characterised in that：Step
（4）The preparation method of the chitosan solution is by chitosan and water in mass ratio 1：200~1：300 mixing, are used in combination acetic acid tune
PH to 4.0~4.2 is saved, chitosan solution is obtained.
7. a kind of preparation method of the special antistatic agent of polyurethane plastics according to claim 1, it is characterised in that：Step
（5）The silane coupling agent is silane resin acceptor kh-550, arbitrary in silane coupling agent KH-560 or Silane coupling reagent KH-570
It is a kind of.
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