CN105820374A - Preparation method of internal mixing antistatic agent and antistatic agent prepared through same - Google Patents
Preparation method of internal mixing antistatic agent and antistatic agent prepared through same Download PDFInfo
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- CN105820374A CN105820374A CN201610237583.9A CN201610237583A CN105820374A CN 105820374 A CN105820374 A CN 105820374A CN 201610237583 A CN201610237583 A CN 201610237583A CN 105820374 A CN105820374 A CN 105820374A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
Abstract
The invention relates to a preparation method of an internal mixing antistatic agent and an antistatic agent prepared through the method. The preparation method comprises the following steps: a, mixing zinc powder with a weak oxidizing solution, and then sequentially carrying out stirring, leaving to stand and drying, so as to obtain a first product; b, mixing the first product obtained in the step a with active carbon, and then performing high-temperature reaction, so as to obtain a second product; c, mixing the second product obtained in the step b, a coupling agent and solvent, heating the mixture to be 50 to 70 DEG C under stirring for reaction for 2 to 6 hours, so as to obtain a third product; d, leaving the third product obtained in the step c to stand for 1 to 3 hours, and then sequentially performing vacuum filtration and vacuum drying, so as to obtain the internal mixing antistatic agent, wherein the coupling agent adopts a silane coupling agent, the the solvent adopts an organic solvent, and the temperature for vacuum drying is 60 to 80 DEG C. After a PET material is blended and internally mixed with the antistatic agent prepared through the method. The surface resistivity of the PET material is obviously reduced, and the antistatic property of the material is obviously improved.
Description
Technical field
The present invention relates to antistatic agent, the preparation method being specifically related to a kind of interior mixed type antistatic agent and the antistatic agent prepared by the method.
Background technology
The positive and negative charge that any object is generally had is equivalent, is that is electroneutral.The mechanisms such as two rubbed, contacts of different objects, electric charge will be moved by contact interface, causes positive excess on one object, and on another object, then negative charge is superfluous, and on interface, form electric double layer, and the space outside two articles does not present electrostatic phenomenon.Make two objects separate when applying any mechanism on this contact interface, then on each object, produce electrostatic respectively, and be externally formed with electrostatic field.Therefore, electrostatic produces through processes such as contact, charge migration, electric double layer formation and separation of charge.When object electrically charged exceed medium in electric field intensity produced by space breakdown strength time, static discharge will occur.Static discharge can become imflammable gas or the incendiary source of dust and set off an explosion and fire.Electrostatic phenomenon polymer production, process and use during be the most universal.Owing to the resistivity of general high polymer is high, the once upper electrostatic of band, just it is difficult to eliminate.The accumulation of these electric charges will be likely to result in the biggest harm, as pharmaceutically drawn dirt, drawing bacterium；Electricity is caused to quiver accident on medical operating；Fire, blast is caused in mine, petrochemical industry；Electronics industry cause integrated circuit destroy；Weaving causes fibril aggregation；In the pipeline being embedded in the various fuel of underground conveying, owing to the flowing of fuel can gather substantial amounts of electrostatic charge on the contact surface of pipeline and fuel；Conveying flammable liquid or the rubber hose of powder body, if one end is equipped with metal tube, can light combustible vapor or powder body due to electrostatic induction and cause fire and explosion accident etc..It is reported, the loss that Electronic Industries causes because of electrostatic charging or electric discharge every year just reaches more than 10,000,000,000 dollars, and the annual rate of growth of the market demand of antistatic product reaches 15%～20%.
Chinese patent CN104419097A discloses a kind of polychloroethylene composition containing composite antistatic agent and preparation method thereof, the described polychloroethylene composition having composite antistatic agent, it is made up of the component of following parts by weight: polyethylene 100 parts, composite antistatic agent 1～5 parts, calcium carbonate 1～3 parts, lubricant 0.8～1.5 parts, described composite antistatic agent is made up of antistatic additive A and antistatic agent B, and weight ratio is: antistatic additive A: antistatic agent B=1:0.2～0.4；Antistatic additive A is Oleum Ricini ethylene oxide condensate, and antistatic agent B is octadecyldimethyl ethoxy quaternary ammonium nitrate, and preparation technology of the present invention is simple, controls easily.After tested, its sheet resistance value is less than 2.5 × 108 Ω, and impact strength is more than 37KJ/m2, for a kind of hard polyethylene compositions with permanence antistatic performance and high impact, and its anti-static function can be kept under any humidity environment.
Chinese patent CN104962011A discloses preparation method and the application of a kind of Compositional type PVC antistatic additive, the preparation of this antistatic additive includes two committed steps: 1, the preparation of fatty acid monoglyceride, esterification feed glycerol and fatty acid react 1～6 hour at 110 DEG C～160 DEG C under the effect of catalyst and get final product；2, the mixing of fatty acid monoglyceride and unclassified stores compounds and i.e. obtains antistatic additive finished product.Described antistatic additive is formed by following material is compounding by weight percentage: fatty acid monoglyceride 50%～80%, polyoxyethylene carboxylate 10%～30%, inorganic metal salt 10%～30%.The PVC antistatic additive of the present invention uses two kinds of nonionic surfactants and inorganic metal salt to compound and obtain, three plays collaborative antistatic property, there is heat resistance preferable, preferable with the PVC matrix compatibility, the features such as cost is relatively low, antistatic property is excellent, has great using value in PVC anti-static material.
The antistatic agent that conventional preparation method prepares is relatively low to the antistatic performance increase rate of material, and the preparation process of antistatic agent is the most complicated.
Summary of the invention
In order to solve the problems referred to above that prior art exists, the preparation method that the invention provides a kind of interior mixed type antistatic agent and the antistatic agent prepared by the method, after banburying being blended by antistatic PET material and the present invention prepared, the surface resistivity of PET material significantly reduces, and the antistatic performance of material reaches to significantly improve.
The technical solution adopted in the present invention is:
A kind of preparation method of interior mixed type antistatic agent, the method includes: a, zinc powder is mixed with weak oxide solution after be stirred successively, stand and be dried, obtain the first product；Wherein, described weak oxide solution be mass concentration be the hydrogen peroxide solution of 0.05-0.2%, hypochlorite solution or liquor natrii hypochloritis；B, the first product of gained in step a is mixed with activated carbon after carry out pyroreaction, obtain the second product；Wherein, the temperature of described pyroreaction is 900-1100 degree Celsius, and the time of pyroreaction is 20-60 minute；C, by the second product of gained in step b, coupling agent and solvent mix after be under agitation heated to 50-70 degree Celsius react 2-6 hour, obtain third product；Wherein, described coupling agent is silane coupler, and solvent is organic solvent；D, gained third product in step c was stood after 1-3 hour carry out vacuum filtration and vacuum drying successively, obtain interior mixed type antistatic agent；Wherein, described vacuum drying temperature is 60-80 degree Celsius.
Preferably, the time stood described in step a is 10-24 hour, and described dry temperature is 100-150 degree Celsius, and the time being dried is 1-2 hour.
Preferably, in step a, the solid-to-liquid ratio of zinc powder and weak oxide solution is 1:(10-200).
Preferably, the mass ratio of the first product and activated carbon described in step b is 1:(0.1-0.7).
Preferably, the mass ratio of the second product, coupling agent and solvent described in step c is 1:(0.01-0.02): (5-50).
Preferably, coupling agent described in step c and solvent are respectively methoxy silane and methanol or respectively Ethoxysilane and ethanol.
Preferably, the pressure of vacuum filtration described in step d is-75～-10 kPas, and the described vacuum drying time is 2-8 hour.
Preferably, the temperature of pyroreaction described in step b is 950-1050 degree Celsius, and the time of pyroreaction is 25-50 minute.
Preferably, the temperature of reacting by heating described in step c is 55-65 degree Celsius, and the time is 2.5-5 hour.
Interior mixed type antistatic agent prepared by preparation in accordance with the present invention.
The invention have the benefit that
One, after banburying being blended by type antistatic agent mixed in preparing with the present invention, the surface resistivity of PET material obtains significantly, the reduction of the order of magnitude, and the antistatic performance of PET material is significantly improved；
Its two, the preparation method of the present invention is simple, it is easy to operation, and used cheaper starting materials is easy to get, applicable industrialized production.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, technical scheme will be described in detail below.Obviously, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, other embodiments all that those of ordinary skill in the art are obtained on the premise of not making creative work, broadly fall into the scope that the present invention is protected.
A kind of preparation method of interior mixed type antistatic agent, the method includes: a, zinc powder is mixed with weak oxide solution after be stirred successively, stand and be dried, obtain the first product；Wherein, described weak oxide solution be mass concentration be the hydrogen peroxide solution of 0.05-0.2%, hypochlorite solution or liquor natrii hypochloritis；B, the first product of gained in step a is mixed with activated carbon after carry out pyroreaction, obtain the second product；Wherein, the temperature of described pyroreaction is 900-1100 degree Celsius, and the time of pyroreaction is 20-60 minute；C, by the second product of gained in step b, coupling agent and solvent mix after be under agitation heated to 50-70 degree Celsius react 2-6 hour, obtain third product；Wherein, described coupling agent is silane coupler, and solvent is organic solvent；D, gained third product in step c was stood after 1-3 hour carry out vacuum filtration and vacuum drying successively, obtain interior mixed type antistatic agent；Wherein, described vacuum drying temperature is 60-80 degree Celsius.
According to the present invention, the time stood described in step a can be 10-24 hour, and described dry temperature can be 100-150 degree Celsius, and the time being dried can be 1-2 hour.
According to the present invention, in step a, zinc powder can be 1:(10-200 with the solid-to-liquid ratio of weak oxide solution).
According to the present invention, the mass ratio of the first product and activated carbon described in step b can be 1:(0.1-0.7).
According to the present invention, the mass ratio of the second product, coupling agent and solvent described in step c can be 1:(0.01-0.02): (5-50).
It is well-known to those skilled in the art according to the present invention, coupling agent and solvent, for example, it is possible to respectively methoxy silane and methanol or respectively Ethoxysilane and ethanol.
Being well-known to those skilled in the art according to the present invention, vacuum filtration and vacuum drying, the such as pressure of vacuum filtration described in step d can be-75～-10 kPas, and the described vacuum drying time can be 2-8 hour.
According to the present invention, the temperature of pyroreaction described in step b can be 950-1050 degree Celsius, and the time of pyroreaction can be 25-50 minute.
According to the present invention, the temperature of reacting by heating described in step c can be 55-65 degree Celsius, and the time can be 2.5-5 hour.
The present invention also provides for the interior mixed type antistatic agent prepared by preparation in accordance with the present invention.
The present invention will be further illustrated by embodiment below, but the present invention is not therefore subject to any restriction.
The intrinsic viscosity of the PET pellet selected by the present invention is 0.8dl/g, and density is 1.3g/cm3。
Surface resistivity is measured by GB/T1410-1989, and instrument is ZC36 type megger.
Embodiment 1
A, according to solid-to-liquid ratio be stirred successively after zinc powder is mixed by 1:10 with the hydrogen peroxide solution that mass concentration is 0.05%, stand 10 hours and 100 degrees Celsius be dried 1 hour, obtain the first product；B, it is to carry out pyroreaction after the first product of gained in step a is mixed with activated carbon by 1:0.1 according to mass ratio, obtains the second product；Wherein, the temperature of described pyroreaction is 900 degrees Celsius, and the time of pyroreaction is 20 minutes；C, it is that 1:0.01:5 reacts being under agitation heated to 50 degrees Celsius after the second product of gained in step b, methoxy silane and methanol mixed 2 hours according to mass ratio, obtains third product；D, gained third product in step c is stood carry out successively after 1 hour pressure be-75～kPa vacuum filtration and vacuum drying 2 hours, obtain interior mixed type antistatic agent KJDJ-1；Wherein, described vacuum drying temperature is 60 degrees Celsius.
Embodiment 2
A, according to solid-to-liquid ratio be stirred successively after zinc powder is mixed by 1:200 with the hypochlorite solution that mass concentration is 0.2%, stand 24 hours and 150 degrees Celsius be dried 2 hours, obtain the first product；B, it is to carry out pyroreaction after the first product of gained in step a is mixed with activated carbon by 1:0.7 according to mass ratio, obtains the second product；Wherein, the temperature of described pyroreaction is 1100 degrees Celsius, and the time of pyroreaction is 60 minutes；C, it is to be under agitation heated to 70 degrees Celsius after the second product of gained in step b, Ethoxysilane and ethanol are mixed by 1:0.02:50 to react 6 hours according to mass ratio, obtains third product；D, gained third product in step c is stood carry out vacuum filtration that pressure is-10 kPas and vacuum drying 8 hours after 3 hours successively, obtain interior mixed type antistatic agent KJDJ-2；Wherein, described vacuum drying temperature is 80 degrees Celsius.
Embodiment 3
A, be 1:100 according to solid-to-liquid ratio by zinc powder and 0.1% liquor natrii hypochloritis's mixing after be stirred successively, stand 17 hours and 125 degrees Celsius be dried 1.5 hours, obtain the first product；B, it is to carry out pyroreaction after the first product of gained in step a is mixed with activated carbon by 1:0.4 according to mass ratio, obtains the second product；Wherein, the temperature of described pyroreaction is 1000 degrees Celsius, and the time of pyroreaction is 40 minutes；C, it is that 1:0.015:30 reacts being under agitation heated to 60 degrees Celsius after the second product of gained in step b, methoxy silane and methanol mixed 4 hours according to mass ratio, obtains third product；D, gained third product in step c is stood carry out vacuum filtration that pressure is-45 kPas and vacuum drying 5 hours after 2 hours successively, obtain interior mixed type antistatic agent KJDJ-3；Wherein, described vacuum drying temperature is 70 degrees Celsius.
Application Example 1:
PET pellet is vacuum dried at 120 DEG C 4-5h, being 10% by PET and antistatic agent KJDJ-1 banburying in the blender of torque rheometer according to antistatic agent accounting mass fraction, banburying temperature is 230 DEG C, and rotor speed is 40rpm, the banburying time is 1omin, obtains blend.The blend of preparation is injected into standard specimen in miniature injector, carries out the test of sheet resistance value.Surface resistivity is calculated by following formula:
Surface resistivity=sheet resistance value * 2 π/ln (d2/d1)；
Wherein sheet resistance value is read by megger, and d1 is for measuring electrode diameter, and d2 is shield electrode internal diameter, and charging voltage is 500v, and the charging interval is 15s, and test temperature is (20-22) DEG C, and humidity is (65-70) %.
Application Example 2-3
Application Example 2, Application Example 3 are identical with the condition of Application Example 1, only difference is that, the antistatic agent used is respectively KJDJ-2 and KJDJ-3, and measured surface resistivity is shown in Table 1.
Comparison study example
Identical with the condition of Application Example 1, only difference is that and be added without antistatic agent, the standard specimen making pure PET carries out the mensuration of surface resistivity.
After banburying being blended by antistatic PET material and the present invention prepared, the surface resistivity of PET material significantly reduces, and the antistatic performance of material reaches to significantly improve.
Table 1
Claims (10)
1. the preparation method of a mixed type antistatic agent, it is characterised in that the method includes:
A, zinc powder is mixed with weak oxide solution after be stirred successively, stand and dry
Dry, obtain the first product；Wherein, described weak oxide solution is that mass concentration is
The hydrogen peroxide solution of 0.05-0.2%, hypochlorite solution or liquor natrii hypochloritis；
B, the first product of gained in step a is mixed with activated carbon after carry out pyroreaction,
Obtain the second product；Wherein, the temperature of described pyroreaction is 900-1100 degree Celsius,
The time of pyroreaction is 20-60 minute；
C, by the second product of gained in step b, coupling agent and solvent mix after stirring
Under be heated to 50-70 degree Celsius react 2-6 hour, obtain third product；Wherein, institute
Stating coupling agent is silane coupler, and solvent is organic solvent；
D, gained third product in step c was stood after 1-3 hour carry out vacuum successively
Sucking filtration and vacuum drying, obtain mixed type antistatic agent；Wherein, described vacuum drying
Temperature is 60-80 degree Celsius.
Preparation method the most according to claim 1, it is characterised in that institute in step a
The time stating standing is 10-24 hour, and described dry temperature is 100-150 degree Celsius, dry
The dry time is 1-2 hour.
Preparation method the most according to claim 1, it is characterised in that zinc powder in step a
It is 1:(10-200 with the solid-to-liquid ratio of weak oxide solution).
Preparation method the most according to claim 1, it is characterised in that described in step b
The mass ratio of the first product and activated carbon is 1:(0.1-0.7).
Preparation method the most according to claim 1, it is characterised in that institute in step c
The mass ratio stating the second product, coupling agent and solvent is 1:(0.01-0.02): (5-50).
Preparation method the most according to claim 1, it is characterised in that institute in step c
State coupling agent and solvent is respectively methoxy silane and methanol or respectively Ethoxysilane and second
Alcohol.
Preparation method the most according to claim 1, it is characterised in that institute in step d
Stating the pressure of vacuum filtration for-75～-10 kPas, the described vacuum drying time is 2-8 hour.
Preparation method the most according to claim 1, it is characterised in that institute in step b
The temperature stating pyroreaction is 950-1050 degree Celsius, and the time of pyroreaction is that 25-50 divides
Clock.
Preparation method the most according to claim 1, it is characterised in that add described in step c
The temperature of thermal response is 55-65 degree Celsius, and the time is 2.5-5 hour.
10. mixed type antistatic prepared by the preparation method of any one in claim 1-9
Agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610237583.9A CN105820374A (en) | 2016-04-15 | 2016-04-15 | Preparation method of internal mixing antistatic agent and antistatic agent prepared through same |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610237583.9A CN105820374A (en) | 2016-04-15 | 2016-04-15 | Preparation method of internal mixing antistatic agent and antistatic agent prepared through same |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087391A (en) * | 2013-03-11 | 2013-05-08 | 河南理工大学 | Antistatic polymer blending composition |
| CN103304898A (en) * | 2013-06-24 | 2013-09-18 | 苏州新区佳合塑胶有限公司 | Antistatic flame retardant PP (polypropylene) material |
-
2016
- 2016-04-15 CN CN201610237583.9A patent/CN105820374A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087391A (en) * | 2013-03-11 | 2013-05-08 | 河南理工大学 | Antistatic polymer blending composition |
| CN103304898A (en) * | 2013-06-24 | 2013-09-18 | 苏州新区佳合塑胶有限公司 | Antistatic flame retardant PP (polypropylene) material |
Non-Patent Citations (1)
| Title |
|---|
| 周志颖: ""抗静电PVC材料的研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20160803 |