CN109797553B - Preparation method of antistatic agent - Google Patents
Preparation method of antistatic agent Download PDFInfo
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- CN109797553B CN109797553B CN201910139452.0A CN201910139452A CN109797553B CN 109797553 B CN109797553 B CN 109797553B CN 201910139452 A CN201910139452 A CN 201910139452A CN 109797553 B CN109797553 B CN 109797553B
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Abstract
The invention provides a preparation method of an antistatic agent, which comprises the following raw materials in parts by mass: 5-12% of Gemini surfactant; 2-4% of high molecular weight alkyl alcohol phosphate; 2-4% of low molecular weight alkyl alcohol phosphate; 0.5-2% of alkanyl alcohol polyphosphate; 1 to 8 percent of polyester. The antistatic agent prepared by the invention has good solubility in water, stable prepared product, small foamability, good heat resistance, acid and alkali resistance and good antistatic effect.
Description
Technical Field
The invention belongs to the technical field of textile material production, and particularly relates to a preparation method of an antistatic agent.
Background
With the rapid development of synthetic fibers, the proportion of the synthetic fibers in textiles is larger and more important. Because synthetic fibers have the characteristics of small hygroscopicity, poor conductivity, large friction coefficient and the like, the problems of static electricity and the hazards thereof generated in the manufacturing, processing and consuming processes are increased continuously. In the production process of textiles, static electricity not only causes the mutual winding and flying of fibers, but also machine parts operate abnormally, so that the processing is difficult to carry out. In the using process of the clothes, the static electricity enables the clothes to be easily polluted and adhered to each other, even electric sparks are generated, and the attractiveness and the comfort of the clothes are seriously influenced. In addition, the static electricity generated by the clothes may interfere with the normal operation of the electronic instrument, for example, if the textile used in the hospital operating room is charged with static electricity, the patient may be accidentally injured during the operation. Therefore, antistatic technology of textiles is very important. Fiber materials generate static electricity when subjected to tension, compression, electric field induction, hot air drying, air stream irradiation, and mutual friction, but the mutual friction between fibers is the most dominant cause of static electricity generation. Although technical means such as fiber modification, blending and cross-spinning can be adopted for inhibiting the static phenomenon of the textile, the antistatic finishing of the textile is generally applied due to the characteristics of convenient processing, low cost and wide applicability. The mechanism of action of antistatic finishing is mainly reflected in two aspects, namely, the reduction of the friction between fibersThe surface resistivity, which is the ratio of the potential gradient parallel to the direction of the current on the surface of the material to the current per unit width of the surface, is expressed in ohms (Ω). This type of antistatic technology relies mainly on ionic conduction, which can bring the surface resistivity of the material from 1014—1016Omega is reduced to 108—1010Omega. Secondly, the static dissipation speed is improved. The antistatic agent is applied to the textile by adopting processing modes of spraying, dipping and padding, so that the fiber has antistatic property.
Existing antistatic agents are classified by ionicity as: anionic, cationic, zwitterionic, and nonionic types.
The anionic antistatic agent mainly comprises sulfate ester, phosphate ester and the like. The sulfate salt has good water solubility, can be used as an emulsifier besides an antistatic effect, but is not stable to oxygen and heat, and is difficult to apply to a high-speed high-temperature spinning process.
The cationic antistatic agent mainly comprises various amine salts, quaternary ammonium salts, alkyl imidazoline salts and the like, wherein the quaternary ammonium salts are most widely applied. However, in addition to antistatic agents, many other auxiliary agents are used in sliver-making, spinning and weaving processes, and since cationic antistatic agents are mostly anionic, cationic antistatic agents cannot be used in most cases. In addition, most cationic antistatic agents are nitrogen-containing compounds, so that the cationic antistatic agents are easy to discolor in a high-temperature environment, so that fibers are colored, the dyeing of the fibers and fabrics thereof is influenced, and a textile machine is easy to rust.
The zwitterionic antistatic agents mainly include amino acid type, betaine type and imidazoline type. Similar to cationic surfactants, amphoteric surfactants, because they contain nitrogen, tend to discolor in high temperature environments, coloring fibers, and affecting the coloration of fibers and their fabrics.
The nonionic antistatic agent is mainly polyethylene oxide alkyl ether, polyethylene oxide alkylphenyl ether, fatty acid ester of polyethylene oxide fatty acid ester glycerol, fatty acid ester of sorbitan, ethylene oxide adduct of polyethylene oxide sorbitan fatty acid ester and amine or amide, etc. The nonionic antistatic agent has poor adsorption to fibers, cannot be ionized and has poor antistatic effect, and the nonionic antistatic agent is used together with the ionic antistatic agent as an antistatic component.
Disclosure of Invention
The antistatic agent prepared by the preparation method provided by the invention has the advantages of good water solubility, stable prepared product, small foamability, good heat resistance, acid and alkali resistance, good antistatic effect, relatively simple preparation, easily obtained raw materials and relatively low cost.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of an antistatic agent is characterized by comprising the following steps: the antistatic agent comprises the following raw materials in parts by mass: 5-12% of Gemini surfactant; 2-4% of high molecular weight alkyl alcohol phosphate; 2-4% of low molecular weight alkyl alcohol phosphate; 0.5-2% of alkanyl alcohol polyphosphate; 1-8% of polyester; wherein, the high molecular weight chain alkyl alcohol phosphate ester surfactant is obtained by the reaction of oleyl alcohol polyoxyethylene ether and phosphorus pentoxide; the low molecular weight chain alkyl alcohol phosphate adopts monolauryl phosphate; the chain alkyl alcohol polyphosphate is obtained by reacting oleyl alcohol polyoxyethylene ether with monolauryl alcohol and polyphosphoric acid.
Further, in the preparation process of the high molecular weight chain alkyl alcohol phosphate surfactant, the feeding molar ratio of the oleyl alcohol polyoxyethylene ether to the phosphorus pentoxide is controlled to be 3-3.5: 1, controlling the reaction temperature at 60-65 ℃, controlling the reaction time at 4-5 hours, adding phosphorus pentoxide into a reaction vessel for 3-5 times, and protecting with nitrogen gas during the reaction.
Further, the preparation of the oleyl alcohol polyoxyethylene ether adopts mixed C14 primary alcohol, C16 primary alcohol and oleyl alcohol as raw materials, and the raw materials are added with ethylene oxide to prepare the mixed fatty alcohol polyoxyethylene ether, wherein the molar ratio of EO to fatty alcohol is 2-3:1, and the mixed molar ratio of C14 primary alcohol, C16 primary alcohol and oleyl alcohol in the raw materials is 0.1-10:0.1-10: 1.
Further, in the preparation process of the alkanyl alcohol polyphosphate, the weight ratio of the oleyl alcohol polyoxyethylene ether, the monolauryl alcohol and the polyphosphoric acid is (2: 1): 1 proportion, and reacting for 4-5 hours at 120 ℃.
Further, the Gemini surfactant has the following structure:
wherein: r3 and R4 are respectively one of dodecyl to eicosyl.
Further, R3 and R4 are heptadecyl groups.
The invention has the advantages and beneficial effects that:
when the oleyl alcohol polyoxyethylene ether reacts with phosphorus pentoxide, the content of the phosphoric monoester is increased along with the prolonging of the reaction time, the content of the phosphoric diester is reduced, the content of the phosphoric acid is reduced, the total acid value is increased, the total conversion rate is improved, and the color and luster of the product are deepened. The phosphate monoester salt is superior to phosphate diester salt in hygroscopicity and antistatic property, and has excellent water solubility. The permeability and smoothness of the phosphate diester salts are better than those of the phosphate monoester salts. This phenomenon is closely related to the structure of the phosphoric acid monoester and diester salt. The phosphate monoester has two O-shaped structures, has stronger hygroscopicity and hydrophilicity than phosphate diester, can better dissipate the charges generated by fiber surface deformation in the weaving process, and has better antistatic effect. The phosphate diester salt has two hydrophobic groups, can form a closely arranged directional adsorption layer on an interface, and has stronger surface tension reduction and capability than the phosphate monoester salt and better permeability. The more phosphate diester salts in the phosphorylated product, the better the product permeability, and the more phosphate monoester salts, the better the product solubility. The electric resistance and permeability of the pyrophosphate salt are poor, and the product performance is seriously influenced by too high content. The reaction time of the invention is controlled between 4 and 5 hours.
According to the invention, the low molecular weight chain alkyl alcohol phosphate monolauryl phosphate is added and added simultaneously with the high molecular weight chain alkyl alcohol phosphate, so that the stability is improved, the viscosity can be reduced, the micromolecules and the fiber surface have better combination effect, fine fiber yarns have better antistatic effect, and the synergistic antistatic effect is achieved when the micromolecules and the high molecular weight phosphate are added simultaneously.
In the invention, the chain alkyl alcohol polyphosphate is added, and is obtained by reacting oleyl alcohol polyoxyethylene ether, monolauryl alcohol and polyphosphoric acid, the obtained polyphosphate has a plurality of hydrophobic chains with different lengths, can be effectively dispersed on the surface of a fiber and improves the bonding strength by virtue of the structure, and meanwhile, the polyphosphoric acid has active groups after partial hydrolysis, has high hydrophilicity and stronger crosslinking performance. The added chain alkyl alcohol polyphosphate synergistically improves the antistatic effect of the high molecular weight chain alkyl alcohol phosphate.
The reason for adopting the Gemini surfactant in the invention is as follows: the Gemini surfactant has high surface activity, and the molecular structure of a classical surfactant is an asymmetric 'amphiphilic' structure formed by a hydrophilic group and a hydrophobic group. The Gemini surfactant (which is called as a dual or twin surfactant in China) has a special structure, and the molecule of the Gemini surfactant at least contains two hydrophilic groups (ions or polar groups) and two hydrophobic chains, and the hydrophilic groups or the positions close to the hydrophilic groups are linked together through chemical bonds by linking groups.
The Gemini surfactant has high surface activity, low Krafft point and good water solubility, contains more hydrophilic and lipophilic groups than the traditional surfactant, can generate stronger synergistic effect when being compounded with the traditional surfactant, and has better effect than the traditional surfactant as an antistatic agent.
When Gemini surfactant molecules are adsorbed on the fiber interface, the lipophilic group faces to the fiber, and the hydrophilic group faces to the air, so that the ion conductivity and the moisture absorption conductivity of the fiber are very strong, namely, a discharge phenomenon is generated, the resistance on the surface of the fiber is reduced, the generation and the release of fiber static electricity are balanced, the static accumulation of the fiber is prevented, and the antistatic purpose is achieved.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Any modifications that can be easily made by a person skilled in the art to the present invention without departing from the technical solutions of the present invention will fall within the scope of the claims of the present invention.
Examples 1 to 3 and comparative examples 1 to 6
12 parts of Gemini surfactant (the specific name of Ningbo east Yongning chemical technology Co., Ltd.: amphoteric Gemini phosphate surfactant), wherein the Gemini surfactant has the following structure:
wherein: r3 and R4 are heptadecyl.
The preparation method of the high molecular weight chain alkyl alcohol phosphate comprises the following steps: the feeding molar ratio of the oleyl alcohol polyoxyethylene ether (C16 primary alcohol polyoxyethylene ether) to the phosphorus pentoxide is controlled to be 3.5: 1, controlling the reaction temperature at 62 ℃ and the reaction time at 5 hours, adding phosphorus pentoxide into a reaction vessel in 4 times, and protecting the reaction vessel by nitrogen gas during the reaction. The preparation of the oleyl alcohol polyoxyethylene ether adopts mixed C14 primary alcohol, C16 primary alcohol and oleyl alcohol with the molar ratio of 1:1:1 as raw materials, and is added with ethylene oxide to prepare the mixed fatty alcohol polyoxyethylene ether, wherein the molar ratio of EO to fatty alcohol is 2.5: 1. In the preparation process of the chain alkyl alcohol polyphosphate, the weight ratio of the oleyl alcohol polyoxyethylene ether, the monolauryl alcohol and the polyphosphoric acid is (2: 1): 1 proportion and reacting for 4 hours at 120 ℃.
The antistatic agent comprises the following components in parts by weight:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Gemini surfactant | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 |
| High molecular weight alkyl alcohol phosphate | 3 | 2 | 4 | 3 | 3 | 3 | 3 | 3 | 3 |
| Monolauryl phosphate | 3 | 2 | 4 | 3 | 3 | 3 | 0 | 5 | 1 |
| Alkanol polyphosphate | 1.5 | 2 | 1 | 0 | 3 | 0.5 | 1.5 | 1.5 | 1.5 |
| Polyester | 4 | 4 | 4 | 4 | 4 | 4 | 4 | 4 | 4 |
| Water (W) | 80 | 80 | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
Antistatic test method
Processing the fabric: bristle polar fleece (Terylene)
The dosage and the process of the antistatic agent are as follows: padding by 20g/L, padding by two times, and drying at 150 ℃.
Washing standard: GB/T8629-2001, washing 5 times by 5A method, hanging and airing each time, and testing half-life period according to test standard GB/T12703.1-2008.
Testing an instrument: FY342E-IIA fabric induction type electrostatic instrument
Raw cloth:
| peak voltage (V) | Decaying voltage (V) | Decay time (S) | |
| Original cloth | 6409 | 3204 | 62.64 |
After antistatic treatment and before washing:
| peak voltage (V) | Decaying voltage (V) | Decay time (S) | |
| Example 1 | 1966 | 983 | 2.58 |
| Example 2 | 2210 | 1105 | 2.32 |
| Example 3 | 3205 | 1603 | 1.23 |
| Comparative example 1 | 3966 | 1983 | 3.36 |
| Comparative example 2 | 4125 | 2063 | 3.03 |
| Comparative example 3 | 4698 | 2349 | 2.28 |
| Comparative example 4 | 4589 | 2295 | 5.3 |
| Comparative example 5 | 4832 | 2416 | 5.2 |
| Comparative example 6 | 3998 | 1999 | 3.1 |
Washing for 5 times after antistatic treatment:
| peak voltage (V) | Decaying voltage (V) | Decay time (S) | |
| Example 1 | 5117 | 2559 | 8.6 |
| Example 2 | 5205 | 2602 | 6.9 |
| Example 3 | 5817 | 2908 | 8.2 |
| Comparative example 1 | 6012 | 3006 | 12.2 |
| Comparative example 2 | 6244 | 3122 | 11.6 |
| Comparative example 3 | 6391 | 3196 | 17.5 |
| Comparative example 4 | 6879 | 3439 | 10.5 |
| Comparative example 5 | 6635 | 3318 | 13.3 |
| Comparative example 6 | 6328 | 3164 | 14.7 |
The above-mentioned embodiments are merely illustrative of the composition and process features of the present system, and are intended to enable those skilled in the art to understand the present invention and implement the present invention, and not to limit the scope of the present invention. The technical solutions formed by the present system or the equivalent substitution method should fall within the protection scope of the claims of the present invention.
Claims (6)
1. A preparation method of an antistatic agent is characterized by comprising the following steps: the antistatic agent comprises the following raw materials in parts by mass: 5-12% of Gemini surfactant; 2-4% of high molecular weight alkyl alcohol phosphate; 2-4% of low molecular weight alkyl alcohol phosphate; 0.5-2% of alkanyl alcohol polyphosphate; 1-8% of polyester; wherein, the high molecular weight chain alkyl alcohol phosphate ester surfactant is obtained by the reaction of oleyl alcohol polyoxyethylene ether and phosphorus pentoxide; the low molecular weight chain alkyl alcohol phosphate adopts monolauryl phosphate; the chain alkyl alcohol polyphosphate is obtained by reacting oleyl alcohol polyoxyethylene ether with monolauryl alcohol and polyphosphoric acid; during the preparation process, the low molecular weight alkyl alcohol phosphate is added simultaneously with the high molecular weight alkyl alcohol phosphate.
2. The process for the preparation of antistatic agents according to claim 1, characterized in that: in the preparation process of the high molecular weight chain alkyl alcohol phosphate surfactant, the feeding molar ratio of the oleyl alcohol polyoxyethylene ether to the phosphorus pentoxide is controlled to be 3-3.5: 1, controlling the reaction temperature at 60-65 ℃, controlling the reaction time at 4-5 hours, adding phosphorus pentoxide into a reaction vessel for 3-5 times, and protecting with nitrogen gas during the reaction.
3. The process for the preparation of antistatic agents according to claim 1, characterized in that: the preparation of the oleyl alcohol polyoxyethylene ether adopts mixed C14 primary alcohol, C16 primary alcohol and oleyl alcohol as raw materials, and is added with ethylene oxide to prepare the mixed fatty alcohol polyoxyethylene ether, wherein the molar ratio of EO to fatty alcohol is 2-3:1, and the mixed molar ratio of C14 primary alcohol, C16 primary alcohol and oleyl alcohol in the raw materials is 0.1-10:0.1-10: 1.
4. The process for the preparation of antistatic agents according to claim 1, characterized in that: in the preparation process of the chain alkyl alcohol polyphosphate, the weight ratio of the oleyl alcohol polyoxyethylene ether, the monolauryl alcohol and the polyphosphoric acid is (2: 1): 1 proportion, and reacting for 4-5 hours at 120 ℃.
5. The process for the preparation of antistatic agents according to claim 1, characterized in that: the structure of the Gemini surfactant is as follows:
wherein: r3、R4Each of dodecyl to eicosyl.
6. The method for preparing an antistatic agent according to claim 5, characterized in that: r3、R4Is heptadecyl.
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Citations (5)
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|---|---|---|---|---|
| US4296165A (en) * | 1978-04-24 | 1981-10-20 | The Diversey Corporation | Antistatic natural and synthetic textile materials which have been treated with salts of orthophosphoric or polyphosphoric acid |
| JP2008255518A (en) * | 2007-04-04 | 2008-10-23 | Es Fibervisions Co Ltd | Antibacterial/deodorizing fiber, fibrous formed article and textile product by using the same |
| KR20140044460A (en) * | 2012-10-05 | 2014-04-15 | 주식회사 피.와이.씨 | Antistatic agent for wool spinning |
| CN106400482A (en) * | 2016-08-30 | 2017-02-15 | 苏州万隆汽车零部件股份有限公司 | Oil agent for improving friction coefficient stability of automotive upholstery fabric |
| CN109371674A (en) * | 2018-09-11 | 2019-02-22 | 杭州传化精细化工有限公司 | A kind of preparation method of textile antistatic agent |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392458B (en) * | 2008-01-30 | 2011-11-30 | 杭州传化化学品有限公司 | Terylene FDY oil and preparation method thereof |
| CN103215806B (en) * | 2013-04-27 | 2014-12-31 | 杭州传化精细化工有限公司 | Antistatic agent for fabrics |
| CN103741465B (en) * | 2013-12-11 | 2016-06-22 | 江阴市尼美达助剂有限公司 | The preparation method of antistatic additive |
| CN105088772A (en) * | 2015-08-13 | 2015-11-25 | 太仓市隆纺油剂有限公司 | Environmentally-friendly anti-yellowing polyester DTY oiling agent and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4296165A (en) * | 1978-04-24 | 1981-10-20 | The Diversey Corporation | Antistatic natural and synthetic textile materials which have been treated with salts of orthophosphoric or polyphosphoric acid |
| JP2008255518A (en) * | 2007-04-04 | 2008-10-23 | Es Fibervisions Co Ltd | Antibacterial/deodorizing fiber, fibrous formed article and textile product by using the same |
| KR20140044460A (en) * | 2012-10-05 | 2014-04-15 | 주식회사 피.와이.씨 | Antistatic agent for wool spinning |
| CN106400482A (en) * | 2016-08-30 | 2017-02-15 | 苏州万隆汽车零部件股份有限公司 | Oil agent for improving friction coefficient stability of automotive upholstery fabric |
| CN109371674A (en) * | 2018-09-11 | 2019-02-22 | 杭州传化精细化工有限公司 | A kind of preparation method of textile antistatic agent |
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