CN112142608A - Antistatic agent and preparation method thereof - Google Patents

Antistatic agent and preparation method thereof Download PDF

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Publication number
CN112142608A
CN112142608A CN202011070436.XA CN202011070436A CN112142608A CN 112142608 A CN112142608 A CN 112142608A CN 202011070436 A CN202011070436 A CN 202011070436A CN 112142608 A CN112142608 A CN 112142608A
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antistatic agent
heating
fatty amine
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汪锋平
郑晓虎
柳岸俊
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Hangzhou Lin'an Dechang Electrostatic Technology Co ltd
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Hangzhou Lin'an Dechang Electrostatic Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/04Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/08Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions not involving the formation of amino groups, hydroxy groups or etherified or esterified hydroxy groups
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C215/00Compounds containing amino and hydroxy groups bound to the same carbon skeleton
    • C07C215/02Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
    • C07C215/04Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being saturated
    • C07C215/06Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being saturated and acyclic
    • C07C215/12Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being saturated and acyclic the nitrogen atom of the amino group being further bound to hydrocarbon groups substituted by hydroxy groups
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/16Anti-static materials

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Abstract

The application relates to the field of additives, and particularly discloses an antistatic agent and a preparation method thereof. The preparation method of the antistatic agent comprises the following steps: firstly, heating C in nitrogen atmosphere with pressure of 0.15-0.2Mpa8‑C12Heating the fatty amine at the temperature of 140 ℃ and 150 ℃, dropwise adding ethylene oxide in a spraying manner while heating the fatty amine, reacting for 1-3h, then aging, and cooling to obtain hydroxyethyl fatty amine; then, mixing hydroxyethyl fatty amine with a solvent, heating to 80-120 ℃, then dropwise adding hydrochloric acid, reacting for 1-3h, cooling, discharging and packaging to obtain the antistatic agent. The preparation method has the advantage of being capable of improving the yield of the antistatic agent.

Description

Antistatic agent and preparation method thereof
Technical Field
The application relates to the field of additives, in particular to an antistatic agent and a preparation method thereof.
Background
Static electricity is common in the production, processing and use processes of polymers, and static electricity accumulation affects the use performance of polymer products, causes dust absorption to damage the appearance, electric shock and even causes explosion phenomena due to sparks generated by static discharge. Antistatic agents are additives that are added to polymers or applied to the surface of polymeric articles to reduce static buildup. Antistatic agents can increase the conductivity of the material, destroy the insulation of the material, and facilitate the rapid leakage or elimination of static charge on the insulation.
Quaternary ammonium salts are a common cationic antistatic agent, and are mostly synthesized by quaternization of tertiary amines with alkylating agents. The tertiary amine is usually prepared by a fatty acid method, which comprises the steps of firstly synthesizing fatty nitrile by using fatty acid, then reacting the fatty nitrile with hydrogen to prepare primary amine, and finally reacting the primary amine with formic acid and formaldehyde to synthesize the tertiary amine. The process for preparing tertiary amines is cumbersome and complex and produces toxic substances. In the reaction process of the tertiary amine and the alkylating reagent, an organic solvent and a catalyst are generally required to be introduced, after the reaction is finished, the organic solvent and the catalyst are removed, and then the product is recrystallized and dried to obtain a powdery solid.
At present, the reaction process of the antistatic agent prepared by the process is complicated, and a certain byproduct is generated, so that the yield of the antistatic agent is low.
Disclosure of Invention
In order to improve the yield of the antistatic agent, the application provides the antistatic agent and the preparation method thereof.
In a first aspect, the present application provides a method for preparing an antistatic agent, which adopts the following technical scheme:
a method for preparing an antistatic agent, comprising the steps of:
step 1: heating C in nitrogen atmosphere with pressure of 0.15-0.2Mpa8-C12Heating the fatty amine at the temperature of 140 ℃ and 150 ℃, dropwise adding ethylene oxide in a spraying manner while heating the fatty amine, reacting for 1-3h, then aging, and cooling to obtain hydroxyethyl fatty amine;
step 2: and (2) mixing hydroxyethyl fatty amine with a solvent, heating to 80-120 ℃, then dropwise adding hydrochloric acid, reacting for 1-3h, cooling to 40-60 ℃, discharging and packaging to obtain the antistatic agent.
By adopting the technical scheme, the fatty amine and the ethylene oxide react at the temperature of 140-150 ℃, the color of the product does not turn yellow, and the transparency is high.
Compared with the traditional solid powdery antistatic agent, the liquid antistatic agent has the advantages that the liquid antistatic agent is in a liquid state within the temperature range of 40-60 ℃, and in the aspect of preparation process, the liquid antistatic agent does not need to be recrystallized and dried, so that the preparation process can be reduced, and the production efficiency can be improved; in addition, the product is in a liquid state, when the antistatic agent is used, the antistatic agent does not need to be dissolved, and the convenience in using the antistatic agent can be improved.
Compared with the traditional method of the antistatic agent, no catalyst is used in the preparation process of the product, so that other materials can be prevented from being introduced, and the purity of the product can be further ensured.
Preferably, the fatty amine accounts for 30-40% by weight; 10-20% of ethylene oxide; 20-30% of hydrochloric acid; 30-40% of solvent.
Preferably, in the step 2, the mass ratio of the hydroxyethyl fatty amine to the solvent is 0.8-1.2: 1.
Preferably, the fatty amine is dodecylamine.
Preferably, the solvent is water.
By adopting the technical scheme, after the reaction is finished, the solvent removal treatment of the product is not needed, the preparation process can be reduced, and the preparation efficiency is improved; meanwhile, the existence of impurities can be reduced, and the purity of the product is improved.
Preferably, in the step 1, the heating rate of heating the fatty amine is 1-3 ℃/min.
Preferably, in the step 1, the dropping rate of the ethylene oxide is 230-270 kg/h.
Preferably, the aging time in the step 1 is 0.5-1.5h, the aging temperature is 140-150 ℃, and the aging pressure is 0.12-1 Mpa.
Preferably, in the step 2, the concentration of the hydrochloric acid is 35-39mol/L, and the dropping rate is 130-170L/h.
Through adopting above-mentioned technical scheme, under this concentration and this dropwise add speed, can avoid the reaction too violent, and then guarantee reaction vessel's security.
In a second aspect, the present application provides an antistatic agent prepared by the above preparation method.
In summary, the present application has the following beneficial effects:
1. the preparation method of the antistatic agent is simple, and compared with the traditional preparation method of the antistatic agent, the hydrochloric acid is acidic, and a catalyst and other additives do not need to be added, so that the residual catalyst and other additives in the reaction process do not need to be removed after the reaction is finished, and the purity and the production efficiency of the product can be improved.
2. The adding mode of hydrochloric acid is a dropwise adding mode, the hydrochloric acid can fully react with hydroxyethyl fatty amine, byproducts are reduced, the reaction effect can be improved, meanwhile, the generation of impurities can be reduced, and the yield of the antistatic agent can be improved.
3. The hydrochloric acid is used as a raw material, so that the reaction cost can be reduced.
4. In the reaction process, water is used as a solvent, so that the method is green and environment-friendly; in addition, after the reaction is finished, solvent removal treatment is not needed, so that the product purity can be improved, and the cost can be reduced.
5. Compared with the traditional preparation method of the antistatic agent, the product does not need recrystallization and drying treatment, and the process steps are reduced; in addition, traditional antistatic agent is powdered, and this product is liquid form, when using this product, need not dissolve this product, convenience when can promoting this product of use.
Detailed Description
The present application will be described in further detail with reference to examples.
The quaternary ammonium salt is used as a cationic antistatic agent and has good antistatic effect. However, in the conventional preparation method, first, a fatty acid method or a fatty alcohol method is generally used to prepare tertiary amine, and the fatty acid method first synthesizes fatty nitrile using fatty acid; then, reacting the aliphatic nitrile with hydrogen to prepare primary amine; and finally, the tertiary amine is synthesized by the reaction of primary amine, formic acid and formaldehyde. The process for preparing tertiary amines is cumbersome and complex and produces toxic substances.
In the reaction process of the tertiary amine and the alkylating agent, the tertiary amine and the alkylating agent are subjected to quaternization reaction under the catalytic action of a catalyst by taking methanol, ethanol or isopropanol as a solvent. Wherein the alkylating agent consists essentially of a halide such as CH3Cl、CH3Br、CH2=CHCH2Cl, aromatic halides such as C6H5CH2Cl、C6H5Cl, dialkyl sulfates, and the like. Because the catalyst and the solvent are introduced in the reaction process, after the reaction is finished, the solvent and the catalyst need to be removed, and then the product is recrystallized and dried to obtain a powdery solid. The process has the disadvantages of multiple steps, complex operation and low working efficiency. In addition, the alkylating agents are costly.
Based on the present discovery, the applicant firstly uses fatty amine and ethylene oxide to prepare hydroxyethyl fatty amine, and obtains transparent hydroxyethyl fatty amine without adding a catalyst by adjusting the reaction time and the reaction temperature. The raw materials needed in the reaction process are few in variety, the process steps are few, the operation is simple, the product purity is high, and the catalyst does not need to be removed. Then, hydrochloric acid is dropwise added to enable the hydrochloric acid to react with the hydroxyethyl fatty amine, so that the reaction effect of the hydrochloric acid and the hydroxyethyl fatty amine can be improved, and the yield is improved; meanwhile, hydrochloric acid reacts with hydroxyethyl fatty amine, so that the generation of impurities can be reduced, and the yield of the antistatic agent is further improved; meanwhile, the product has high transparency, and the aesthetic property of the high polymer product is not influenced after the antistatic agent is applied to the high polymer product. In addition, the cost of the hydrochloric acid is low.
The following comparative examples and examples:
the dodecylamine is produced by Hangzhou Jun chemical industry Co.Ltd;
ethylene oxide was produced by Tenmour Industrial and trade company, Inc., of Cian.
Examples
Example 1
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; adding 3000kg of dodecylamine into a reaction kettle, vacuumizing the reaction kettle after feeding is finished, supplementing nitrogen, and adjusting the pressure of the reaction kettle to be 0.2 Mpa;
step 2: heating dodecylamine to 150 ℃ at a heating rate of 1 ℃/min, dropwise adding ethylene oxide at a dropping rate of 230kg/h in a spray dropping manner while heating fatty amine, wherein the total weight of 2000kg, and then reacting the fatty amine with the ethylene oxide for 1h to obtain the dodecyl diethoxyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: c is to be12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2Aging under 0.12Mpa at 150 deg.C for 0.5h, and cooling to make the reaction more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 1.2:1, heating to 80 ℃, then dripping 3000kg of hydrochloric acid with the concentration of 35mol/L at the dripping speed of 170L/h, reacting for 1h, cooling to 60 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
example 2
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; 4000kg of dodecylamine is added into a reaction kettle, the reaction kettle is vacuumized after the feeding is finished, nitrogen is supplemented, and the pressure of the reaction kettle is adjusted to be 0.15 Mpa;
step 2: heating dodecylamine to 140 ℃ at a heating rate of 3 ℃/min, dropwise adding ethylene oxide at a dropping rate of 270kg/h in a spray dropwise adding mode while heating fatty amine, and then reacting the fatty amine with the ethylene oxide for 3h to obtain the dodecyl dihydroxyethyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: aging the product obtained in the step 2 for 1.5h under the conditions that the pressure is 1Mpa and the temperature is 140 ℃, and then cooling to ensure that the reaction is more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 0.8:1, heating to 120 ℃, then dripping 2000kg of hydrochloric acid with the concentration of 39mol/L at the dripping speed of 130L/h, reacting for 3h, cooling to 40 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
example 3
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; 3500kg of dodecylamine is added into the reaction kettle, the reaction kettle is vacuumized after the feeding is finished, nitrogen is supplemented, and the pressure of the reaction kettle is adjusted to be 0.17 Mpa;
step 2: heating dodecylamine to 145 ℃ at a heating rate of 2 ℃/min, dripping ethylene oxide at a dripping rate of 250kg/h in a spray dripping mode while heating fatty amine to obtain 1500kg, and reacting the fatty amine with the ethylene oxide for 2h to obtain the dodecyl dihydroxyethyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: aging the product obtained in the step 2 for 1h under the conditions that the pressure is 0.6Mpa and the temperature is 145 ℃, and then cooling to ensure that the reaction is more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 1:1, heating to 100 ℃, then dripping hydrochloric acid with the concentration of 37mol/L at the dripping speed of 150L/h for 2500kg, reacting for 2h, cooling to 50 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
example 4
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; 3200kg of dodecylamine is added into the reaction kettle, the reaction kettle is vacuumized after the feeding is finished, nitrogen is supplemented, and the pressure intensity of the reaction kettle is adjusted to be 0.19 Mpa;
step 2: heating dodecylamine to 147 ℃ at the heating rate of 1.5 ℃/min, heating fatty amine while dropwise adding ethylene oxide at the dropping rate of 240kg/h in a spray dropwise adding mode, and then reacting the fatty amine with the ethylene oxide for 2.5h to obtain the dodecyl dihydroxyethyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: aging the product obtained in the step 2 for 1.25h under the conditions that the pressure is 0.8Mpa and the temperature is 142 ℃, and then cooling to ensure that the reaction is more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 0.9:1, heating to 110 ℃, then dropwise adding hydrochloric acid with the concentration of 38mol/L at the dropwise adding rate of 140L/h to reach 2300kg, reacting for 2.5h, cooling to 45 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
example 5
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; 3700kg of dodecylamine is added into the reaction kettle, the reaction kettle is vacuumized after the feeding is finished, nitrogen is supplemented, and the pressure of the reaction kettle is adjusted to be 0.16 Mpa;
step 2: heating dodecylamine to 142 ℃ at a heating rate of 2.5 ℃/min, heating fatty amine while dropwise adding ethylene oxide at a dropping rate of 260kg/h in a spray dropping manner to obtain 1700kg of ethylene oxide, and reacting the fatty amine with the ethylene oxide for 1.5h to obtain the dodecyl dihydroxyethyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: aging the product obtained in the step (2) for 0.7h under the conditions that the pressure is 0.14Mpa and the temperature is 147 ℃, and then cooling to ensure that the reaction is more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 1.1:1, heating to 90 ℃, then dripping 36mol/L hydrochloric acid at the dripping speed of 160L/h for 2700kg, reacting for 1.2h, cooling to 55 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
comparative example
Comparative example 1
In contrast to example 3, no water was added in step 4.
Comparative example 2
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; 3500kg of dodecylamine is added into the reaction kettle, the reaction kettle is vacuumized after the feeding is finished, nitrogen is supplemented, and the pressure of the reaction kettle is adjusted to be 0.17 Mpa;
step 2: heating dodecylamine to 120 ℃ at a heating rate of 2 ℃/min, dripping ethylene oxide at a ventilation dripping rate of 250kg/h in a spray dripping mode while heating fatty amine, and then reacting the fatty amine with the ethylene oxide for 2h to obtain the dodecyl dihydroxyethyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: aging the product obtained in the step 2 for 1h under the conditions that the pressure is 0.6Mpa and the temperature is 120 ℃, and then cooling to ensure that the reaction is more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 1:1, heating to 60 ℃, then dripping hydrochloric acid with the concentration of 37mol/L at the dripping speed of 150L/h for 2500kg, reacting for 2h, cooling to 50 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
comparative example 3
A method for preparing an antistatic agent, comprising the steps of:
step 1: vacuumizing the reaction kettle, supplementing nitrogen, replacing gas twice, and removing water vapor in the reaction kettle; 3500kg of dodecylamine is added into the reaction kettle, the reaction kettle is vacuumized after the feeding is finished, nitrogen is supplemented, and the pressure of the reaction kettle is adjusted to be 0.17 Mpa;
step 2: heating dodecylamine to 145 ℃ at a heating rate of 2 ℃/min, dripping ethylene oxide at a dripping rate of 250kg/h in a spray dripping mode while heating fatty amine to obtain 1500kg, and reacting the fatty amine with the ethylene oxide for 1h to obtain the dodecyl dihydroxyethyl tertiary amine, wherein the reaction equation is as follows:
C12H25NH2+2C2H4O→C12H25N(CH2CH2OH)2
and step 3: aging the product obtained in the step 2 for 0.5h under the conditions that the pressure is 0.6Mpa and the temperature is 145 ℃, and then cooling to ensure that the reaction is more complete;
and 4, step 4: mixing the dodecyl dihydroxyethyl tertiary amine obtained in the step 3 with water according to the mass ratio of 1:1, heating to 100 ℃, then dripping hydrochloric acid with the concentration of 37mol/L at the dripping speed of 150L/h for 2500kg, reacting for 1h, cooling to 50 ℃, discharging and packaging to obtain the antistatic agent, wherein the reaction equation is as follows:
C12H25N(CH2CH2OH)2+HCl→[RNH(CH2CH2OH)(CH2CH2OH)]+Cl-
performance detection
The productivity and antistatic performance of the antistatic agents in examples 1 to 5 and comparative examples 1 to 3 were tested in the following manner.
1) And (3) purity testing: the yield of the antistatic agent was determined by chemical titration according to QB1915-93 cationic surfactant, fatty alkyl dimethyl ammonium halide and fatty alkyl dimethyl benzyl halide.
TABLE 1 yield of antistatic agent
Item Practice ofExample 1 Example 2 Example 3 Example 4 Example 5 Comparative example 1 Comparative example 2 Comparative example 3
Yield (%) 98.8 98.6 99.4 99.2 99.1 91.5 94.3 93.2
As can be seen by combining examples 1-5 and comparative examples 1-3 with Table 1, the antistatic agents prepared by the preparation methods of examples 1-5 all had yields of 98% or more; the productivity of the antistatic agent prepared by the preparation method of the embodiment 3-5 is higher than 99 percent; in comparative example 1, no water was added, and when the tertiary amine conversion rate was high, the viscosity of the reaction system was large, and the quaternization reaction was difficult to proceed, resulting in a low yield of the antistatic agent; while comparative examples 2 and 3 were synthesized under conditions outside the range defined in the present application, the yield of the obtained product was low due to a low reaction temperature or a too short reaction time. Therefore, only by adopting the preparation process and the specific composition and conditions, the raw materials can be fully reacted, and the yield of the product is improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (10)

1. The preparation method of the antistatic agent is characterized by comprising the following steps:
step 1: heating C in nitrogen atmosphere with pressure of 0.15-0.2Mpa8-C12Heating the fatty amine at the temperature of 140 ℃ and 150 ℃, dropwise adding ethylene oxide in a spraying manner while heating the fatty amine, reacting for 1-3h, then aging, and cooling to obtain hydroxyethyl fatty amine;
step 2: and (2) mixing hydroxyethyl fatty amine with a solvent, heating to 80-120 ℃, then dropwise adding hydrochloric acid, reacting for 1-3h, cooling to 40-60 ℃, discharging and packaging to obtain the antistatic agent.
2. The method for preparing an antistatic agent according to claim 1, characterized in that: 30-40% by weight of the fatty amine; 10-20% of ethylene oxide; 20-30% of hydrochloric acid; 30-40% of solvent.
3. The method for preparing an antistatic agent according to claim 1, characterized in that: in the step 2, the mass ratio of the hydroxyethyl fatty amine to the solvent is 0.8-1.2: 1.
4. The method for preparing an antistatic agent according to claim 1, characterized in that: the fatty amine is dodecylamine.
5. The method for preparing an antistatic agent according to claim 1, characterized in that: the solvent is water.
6. The method for preparing an antistatic agent according to claim 1, characterized in that: in the step 1, the heating rate of heating the fatty amine is 1-3 ℃/min.
7. The method for preparing an antistatic agent according to claim 1, characterized in that: in the step 1, the dropping rate of the ethylene oxide is 230-270 kg/h.
8. The method for preparing an antistatic agent according to claim 1, characterized in that: in the step 1, the aging time is 0.5-1.5h, the aging temperature is 140-150 ℃, and the aging pressure is 0.12-1 Mpa.
9. The method for preparing an antistatic agent according to claim 1, characterized in that: in the step 2, the concentration of the hydrochloric acid is 35-39mol/L, and the dropping rate of the hydrochloric acid is 130-170L/h.
10. An antistatic agent prepared according to any one of the preparation methods of claims 1 to 9.
CN202011070436.XA 2020-10-09 2020-10-09 Antistatic agent and preparation method thereof Pending CN112142608A (en)

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顾立敏: "烷基胺的环氧乙烷加成型抗静电剂", 《石油化工》 *

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