CN105778445A - High molecular antistatic agent and preparation method thereof - Google Patents
High molecular antistatic agent and preparation method thereof Download PDFInfo
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—Dicarboxylic acids and dihydroxy compounds
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Abstract
The invention discloses a high molecular antistatic agent and a preparation method thereof. The high molecular antistatic agent is a copolymer which is formed by polymerizing a benzene ring monomer and a polymer, wherein the benzene ring monomer contains sulfo and carboxyl, and the polymer contains a polyether block and a polyamide block; the end groups of the polyether block and the polyamide block are carboxyl; the monomer and the polymer are synthesized into the high molecular polymer under the vacuum condition. The high molecular antistatic agent has the advantages that the durability, heat-resistant property, compatibility and antistatic property are excellent; the high molecular antistatic agent is mainly applied by being added into matrix resin, and is an internal millable type antistatic agent.
Description
Technical field
The invention belongs to macromolecule permanent type antistatic field, be specifically related to a kind of Polymer Antistatic Agent and preparation method thereof.
Background technology
Owing to most of polymer surface resistance or specific insulation are higher, thus there is good insulating properties and be widely used and industry insulant.But in the application because of friction, peeling off or sense process generation and stored charge, bringing very big hidden danger to production safety, the electrostatic charge that timely material for transfer surface produces is the most straightforward approach preventing static discharge from occurring.Industrial usual employing is added the method for antistatic additive and is reached the electrostatic charge that transfer polymer surface produces, thus preventing the generation of static discharge.
Antistatic additive, by the difference of chemical composition, generally can be divided into cationic, anionic, amphoteric ion type, non-ionic and macromolecule permanent type.The antistatic property of cationic antistatic agent is excellent, has microbe killing properties, the performance such as flexibility and emulsibility simultaneously, but poor heat resistance；The thermostability of anionic antistatic agent and antistatic behaviour are all relatively good, but poor with the compatibility of substrate resin, affect its transparency and aesthetic property；The amphoteric ion type antistatic additive compatibility and antistatic effect are better, but thermostability is not as anionic；The compatibility of non-ionic antistatic agent and thermostability are good, however it is necessary that bigger addition；Macromolecule permanent antistatic agent is divided into again hydrophilic macromolecule antistatic additive and intrinsically conducting Polymer-metallic Catalyst, hydrophilic macromolecule antistatic additive will no longer show antistatic effect when humidity is lower than 20%, intrinsically conducting Polymer-metallic Catalyst has the advantages that high molecular abundant structure, machinability and density are little, the antistatic of High Molecular Permanent Antistatic Agent is lasting simultaneously, without induction period, being susceptible to the impact of the condition such as wiping, washing, but addition is relatively big, price is higher.
Summary of the invention
In order to overcome cationic antistatic agent poor heat resistance, the anionic antistatic agent compatibility is not enough, it is maintained with the persistency of macromolecule permanent antistatic agent, reduce its addition and the impact on environment thereof, improve antistatic property, the present invention provides a kind of Polymer Antistatic Agent and preparation method thereof, this antistatic additive not only has the persistency of macromolecule permanent antistatic agent, the structure that macromolecule is abundant, machinability and the little feature of density, and without induction period, it is susceptible to wiping, the impact of the conditions such as washing, there is the excellent thermostability of anionic antistatic agent and excellent antistatic property simultaneously.The ionic thermostability that improve Polymer Antistatic Agent in this type of antistatic additive and antistatic property, the feature of high molecular compensate for again the ionic anti-static agent compatibility and persistent deficiency simultaneously.
Polymer Antistatic Agent of the present invention be the technical scheme is that to design a class high polymer, and the structure of this high polymer includes phenyl ring, sulfonic group, ester bond, Polyethylene Glycol segmented structure, and end group is with hydroxyl.The conjugatedπbond of phenyl ring makes it have intrinsic conductivity, sulfonic acid group makes macromolecule have the feature of ion-type, enhance thermostability and the electric conductivity of macromolecular material, middle Polyethylene Glycol segmented structure adds the compatibility of material, the hydroxyl of end group is hydrophilic group, it is possible to increase antistatic property.
A kind of preparation method of Polymer Antistatic Agent, step is as follows:
1) caprolactam of 100～140 molar part, 30～35 molar part adipic acids, 0.2～0.5 molar part antioxidant KY1010 are added in reaction vessel, after gas in reaction vessel is replaced with nitrogen, at 200～240 DEG C, reaction 3～5h under the pressure of 0.1～0.3MPa, obtain polyamide；
2) be reduced to after room temperature addition 140～180 molar part Polyethylene Glycol until temperature, 200～255 DEG C, lower reaction 3～7h obtain polymerizate；
3) adding the phenyl ring with sulfonic group and carboxyl and Loprazolam, react 1～3h at 200～240 DEG C, secure satisfactory grades subtype antistatic additive.
A kind of preparation method of Polymer Antistatic Agent, the method preparation process is as follows:
1) by 7～15 molar part phenyl ring with sulfonic group and carboxyl, 20～30 molar part Polyethylene Glycol and 1.6～15 molar part Loprazolam mix homogeneously；
2) it is heated at 100～120 DEG C and reacts 1～2h；
3) NaCO is used3Neutralizing, ethanol precipitates, and product dried, secure satisfactory grades subtype antistatic additive.
Further, the described phenyl ring with sulfonate is Sodium Dimethyl Isophthalate-5-sulfonate, 5-sodium sulfo isophthalate, dimethyl isophthalate-5-potassium sulfonate or M-phthalic acid-5-potassium sulfonate.
Further, step 3) 1/2-1/3 that consumption is polymerizate mole of the described phenyl ring with sulfonic acid group.
Further, step 3) described Loprazolam consumption is polymerizate mole 8%～15%.
A kind of Polymer Antistatic Agent prepared by above-described preparation method, this antistatic additive contains benzene ring structure, and wherein, between phenyl ring, there are three substituent groups position.Three substituent groups of position between described phenyl ring, one of them is sulfonic acid group, and other two is polymer segment containing ester bond, ehter bond, amido link and hydroxyl.Described sulfonic acid group is neutralized by alkali metal ion, for potassium ion or sodium ion.Described polymer segment is the product of acylamide polymer and polyethylene glycol polymeric, and the end group of product is hydroxyl, then the carboxyl condensation polymerization of hydroxyl and phenyl ring.Described amide polymer segment is by the product of dicarboxylic acids with the polymerization containing amino.
Polymer Antistatic Agent is to be added in macromolecular material in the way of the interpolation of inside, then processes together with material.
Compared with prior art, the invention have the advantages that and technique effect:
1, the Polymer Antistatic Agent of the present invention has good persistency, thermostability, the compatibility and excellent antistatic property.
2, the Polymer Antistatic Agent of the present invention is without induction period, is susceptible to the impact of the condition such as wiping, washing.
Accompanying drawing explanation
Fig. 1 is the chemical structural formula after adding Polyethylene Glycol after adipic acid and caprolactam polymerization；
Fig. 2 is that adipic acid completes with caprolactam polymerization and add continuation after Polyethylene Glycol reacts to obtain the chemical structural formula of target product after adding SSIPA/SIPM；
Fig. 3 is the thermogravimetric analysis figure of material shown in Fig. 2.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated, but is not limited thereto.
Embodiment 1
The synthetic route of the present embodiment is as follows:
By the 5-sodium sulfo isophthalate (5-SSIPA) of 10 molar part, the Polyethylene Glycol (PEG) of 28 molar part and reaction 1h at the Loprazolam mixing post-heating to 100 DEG C of 10 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition, result is in Table 1.
Table 1
Table 1 illustrates to add after above-mentioned antistatic additive, and polyacrylic volume resistance and sheet resistance reduce notable, has excellent antistatic property, and along with the increase of addition has the trend of reduction further, when addition effect when about 10% is best.
Embodiment 2
By the 5-sodium sulfo isophthalate (5-SSIPA) of 10 molar part, the Polyethylene Glycol (PEG) of 28 molar part and reaction 1h at the Loprazolam mixing post-heating to 120 DEG C of 10 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The M-phthalic acid two macrogol ester-5-sodium sulfonate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 1.
Embodiment 3
By the 5-sodium sulfo isophthalate (5-SSIPA) of 10 molar part, the Polyethylene Glycol (PEG) of 28 molar part and reaction 2h at the Loprazolam mixing post-heating to 120 DEG C of 10 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The M-phthalic acid two macrogol ester-5-sodium sulfonate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 1.
Embodiment 4
By the 5-sodium sulfo isophthalate (5-SSIPA) of 7 molar part, the Polyethylene Glycol (PEG) of 30 molar part and reaction 1h at the Loprazolam mixing post-heating to 120 DEG C of 10 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The M-phthalic acid two macrogol ester-5-sodium sulfonate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 1.
Embodiment 5
By the 5-sodium sulfo isophthalate (5-SSIPA) of 15 molar part, the Polyethylene Glycol (PEG) of 20 molar part and reaction 1h at the Loprazolam mixing post-heating to 120 DEG C of 10 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The M-phthalic acid two macrogol ester-5-sodium sulfonate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 1.
Embodiment 6
By the 5-sodium sulfo isophthalate (5-SSIPA) of 10 molar part, the Polyethylene Glycol (PEG) of 28 molar part and reaction 1h at the Loprazolam mixing post-heating to 120 DEG C of 1.6 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The M-phthalic acid two macrogol ester-5-sodium sulfonate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 1.
Embodiment 7
By the 5-sodium sulfo isophthalate (5-SSIPA) of 10 molar part, the Polyethylene Glycol (PEG) of 28 molar part and reaction 1h at the Loprazolam mixing post-heating to 120 DEG C of 15 molar part, after reaction, use Na2CO3Neutralizing, ethanol precipitates, and product dried obtains M-phthalic acid two macrogol ester-5-sodium sulfonate.Mix with polypropylene (PP) according to the mass ratio that M-phthalic acid two macrogol ester-5-sodium sulfonate/polypropylene is 5%, 10%, 15%, 20%, in mill mixing, tabletting in vulcanizer, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The M-phthalic acid two macrogol ester-5-sodium sulfonate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 1.
Embodiment 8
Synthetic route is as follows:
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mixing with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition, result is in Table 2.
Table 2
Table 2 illustrates to add after above-mentioned antistatic additive, and polyacrylic volume resistance and sheet resistance reduce notable, has excellent antistatic property, and along with the increase of addition has the trend of reduction further, when addition effect when about 20% is best.
Embodiment 9
The polymerizate of embodiment 8 gained adds 96 molar part 5-sodium sulfo isophthalates (5-SSIPA), it is simultaneously introduced the Loprazolam of polymerizate 10mol%, react 2h at 220 DEG C, obtain target product (chemical structural formula is as shown in Figure 2).Above-mentioned target product is carried out thermogravimetric analysis, and result, as it is shown on figure 3, the decomposition temperature of target product is higher as shown in Figure 3, has the feature of thermostability.Mixing with polypropylene (PP) according to the mass ratio that target product/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition, result is in Table 3.
Table 3
Table 3 illustrates to add after above-mentioned antistatic additive, and polyacrylic volume resistance and sheet resistance reduce notable, has excellent antistatic property, and along with the increase of addition has the trend of reduction further, when addition effect when about 15% is best.
Tabletting was placed after 30 days, and test surfaces resistance and volume resistance again under 25 DEG C and 40% damp condition, result is in Table 4.
Table 4
Table 4 illustrates still have excellent antistatic property through placement material for a long time, and therefore the antistatic property of this antistatic additive has persistency.
Embodiment 10
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 200 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 11
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 240 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 12
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 3h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 13
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 5h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 14
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.1MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 15
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.3MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 16
By the caprolactam of 100 molar part, the adipic acid of 35 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 17
By the caprolactam of 140 molar part, the adipic acid of 30 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 18
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 200 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 19
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 255 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 20
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 160 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 3h or 7h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 21
By the caprolactam of 120.2 molar part, the adipic acid of 33.1 molar part, the antioxidant (KY1010) of 0.3 molar part adds in reaction vessel, after being replaced with nitrogen by reaction vessel, at 220 DEG C, reaction 4h under the pressure of 0.2MPa, obtains polyamide.
Add the Polyethylene Glycol of 140 or 180 molar part Mn6000 after being cooled to room temperature, at 240 DEG C, react 5h obtain polymerizate (chemical structural formula is as shown in Figure 1).Mix with polypropylene (PP) according to the mass ratio that polymerizate/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The polymerizate that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 8.
Embodiment 22
The polymerizate of embodiment 8 gained adds 96 molar part 5-sodium sulfo isophthalates (5-SSIPA), it is simultaneously introduced the Loprazolam of polymerizate 10mol%, react 1 or 3h at 220 DEG C, obtain target product (chemical structural formula is as shown in Figure 2).Above-mentioned target product is carried out thermogravimetric analysis, and result, as it is shown on figure 3, the decomposition temperature of target product is higher as shown in Figure 3, has the feature of thermostability.Mix with polypropylene (PP) according to the mass ratio that target product/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The target product that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 9.
Embodiment 23
The polymerizate of embodiment 8 gained adds 96 molar part 5-sodium sulfo isophthalates (5-SSIPA), it is simultaneously introduced the Loprazolam of polymerizate 10mol%, react 2h at 200 DEG C or 240 DEG C, obtain target product (chemical structural formula is as shown in Figure 2).Above-mentioned target product is carried out thermogravimetric analysis, and result, as it is shown on figure 3, the decomposition temperature of target product is higher as shown in Figure 3, has the feature of thermostability.Mix with polypropylene (PP) according to the mass ratio that target product/polypropylene is 5%, 10%, 15%, 20%, mixing in mill, vulcanizer tabletting, test surfaces resistance and volume resistance under 25 DEG C and 40% damp condition.The target product that the present embodiment prepares has excellent antistatic property equally, and concrete outcome is referring to embodiment 9.
Claims (7)
1. the preparation method of a Polymer Antistatic Agent, it is characterised in that step is as follows:
1) caprolactam of 100～140 molar part, 30～35 molar part adipic acids, 0.2～0.5 molar part antioxidant KY1010 are added in reaction vessel, after gas in reaction vessel is replaced with nitrogen, at 200～240 DEG C, reaction 3～5h under the pressure of 0.1～0.3MPa, obtain polyamide；
2) be reduced to after room temperature addition 140～180 molar part Polyethylene Glycol until temperature, 200～255 DEG C, lower reaction 3～7h obtain polymerizate；
3) adding the phenyl ring with sulfonic group and carboxyl and Loprazolam, react 1～3h at 200～240 DEG C, secure satisfactory grades subtype antistatic additive.
2. the preparation method of a kind of Polymer Antistatic Agent according to claim 1, it is characterised in that preparation process is as follows:
1) by 7～15 molar part phenyl ring with sulfonic group and carboxyl, 20～30 molar part Polyethylene Glycol and 1.6～15.0 molar part Loprazolam mix homogeneously；
2) it is heated at 100～120 DEG C and reacts 1～2h；
3) NaCO is used3Neutralizing, ethanol precipitates, and product dried, secure satisfactory grades subtype antistatic additive.
3. the preparation method of a kind of Polymer Antistatic Agent according to claim 1, it is characterized in that, the described phenyl ring with sulfonic group and carboxyl is Sodium Dimethyl Isophthalate-5-sulfonate, 5-sodium sulfo isophthalate, dimethyl isophthalate-5-potassium sulfonate or M-phthalic acid-5-potassium sulfonate.
4. the preparation method of a kind of Polymer Antistatic Agent according to claim 2, it is characterized in that, the described phenyl ring with sulfonic group and carboxyl is Sodium Dimethyl Isophthalate-5-sulfonate, 5-sodium sulfo isophthalate, dimethyl isophthalate-5-potassium sulfonate or M-phthalic acid-5-potassium sulfonate.
5. the preparation method of a kind of Polymer Antistatic Agent according to claim 1, it is characterised in that be step 2 with the consumption of sulfonic group and the phenyl ring of carboxyl described in step 3)) 1/2-1/3 of gained polymerizate mole.
6. the preparation method of a kind of Polymer Antistatic Agent according to claim 1, it is characterised in that the consumption of Loprazolam described in step 3) is step 2) gained polymerizate mole 8%～15%.
7. a kind of Polymer Antistatic Agent that the preparation method described in any one of claim 1-6 prepares.
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| CN108047536A (en) * | 2017-12-20 | 2018-05-18 | 苏州星火丰盈环保包装有限公司 | Degradable antistatic packaging bag and preparation method thereof |
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| CN112442163B (en) * | 2020-11-27 | 2021-11-26 | 上海凯斐服饰有限公司 | Preparation method of high-molecular polyester antistatic agent |
| CN114524922A (en) * | 2022-03-02 | 2022-05-24 | 浙江海正生物材料股份有限公司 | Antistatic modified polylactic acid and preparation method thereof |
| CN114524922B (en) * | 2022-03-02 | 2024-03-22 | 浙江海正生物材料股份有限公司 | Antistatic modified polylactic acid and preparation method thereof |
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| CN115785457A (en) * | 2022-12-02 | 2023-03-14 | 四川苇航高新材料有限公司 | PEO-based permanent antistatic agent and preparation method thereof |
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