CN102586510B - Preparation method for leather greasing agent containing modified graphene oxide - Google Patents
Preparation method for leather greasing agent containing modified graphene oxide Download PDFInfo
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Abstract
The invention relates to a preparation method for a leather greasing agent containing modified graphene oxide. The greasing agent is a leather chemical product with the maximum consumption in the production process. The preparation method comprises the following steps: adding sulfuric acid into graphite powder and sodium nitrate; adding potassium permanganate, washing and carrying out ultrasound to obtain a graphene oxide aqueous solution; dissolving octadecyl dimethyl-2-hydroxyethyl ammonium bromide into absolute ethyl alcohol; adding the mixed solution into a graphene oxide dispersion solution and carrying out ultrasound to obtain graphene oxide and octadecyl dimethyl-2-hydroxyethyl ammonium bromide direct intercalation composition; mixing and reacting oleic acid, methoxy polyethylene glycol 1200 and para-toluenesulfonic acid to obtain oleic acid polyethylene glycol monomethyl ether ester; uniformly stirring the obtain graphene oxide intercalation composition, the oleic acid polyethylene glycol monomethyl ether ester, natural grease, sulfonated oil SS, isopropanol and de-ionized water; and carrying out ultrasonic dispersion to obtain the leather greasing agent. The leather greasing agent disclosed by the invention has an excellent softening effect for leather fiber, the function of improving strength and toughness, and a very high absorption rate; and the dyeing effect of leather is remarkably improved.
Description
Technical field
The present invention relates to a kind of preparation method of leather fat, be specifically related to a kind of preparation method who contains modified oxidized Graphene leather fat.
Background technology
Fatting agent is the leather chemicals of consumption maximum in the leather production process, and the quality of fatting agent is one of principal element that influences leather quality, and the fatting agent of therefore researching and developing ideal performance is one of focus of research always.Fatting agent be by various greases and modified product thereof and suitable tensio-active agent composite form a kind of mixture.At present, leather fat is relatively paid attention to the compound, composite of heterogeneity on component constitutes, at present main leather fat is that the process proper proportion is composite obtains by the modified product of natural fats and oils and Synthetic Oil and tensio-active agent, functional aid etc., mainly be to reach maximizing favourable factors and minimizing unfavourable ones on the performance by composite, show synergistic effect, improve the stuffing effect; On performance, pay attention to having certain specific character or function, promptly in stuffing, can have certain function concurrently,, make the stuffing leather more can satisfy human consumer's needs as functions such as filling, retanning, mercerising, waterproof, fire-retardant, perfuming, anti-enzymes.The graphene oxide development function type leather fat potentiality that utilization has excellent properties are very big.
Graphene oxide has performances such as superstrength, superelevation snappiness, super large specific surface area, excellent electrical and thermal conductivity performance and surperficial alternative functionalization because of it makes it become one of current most popular material, and strengthening toughness reinforcing, opto-electronic device, motor material and catalytic field at macromolecular material has huge application potential.Although the research of nano graphene oxide in these fields is the focus of studying both at home and abroad at present; but apart from mass-producing use also have suitable remote; reason is a kind of means that graphene oxide is just realized nano-dispersed in these fields, and reduction reaction subsequently and nano level under anhydrous state disperse to be one and temporarily be difficult to the thing accomplished.And the currying work of in water medium, carrying out, the Heaven-sent chance of in water, being dispersed into the nano level lamella and entering leather fiber by water medium for graphene oxide.What therefore, really have a mass-producing application prospect is to use nano graphene oxide in water medium.Graphene oxide has super large specific surface area nano laminated structure, contain hydroxyl, carboxyl and epoxy group(ing) isoreactivity group on the surface, have good hydrophilicity energy and certain surfactivity, can enter leather fiber by water medium and form nanocomposite with it, manifest the effect of softening leather fiber, form the network cross-linked structure and have the toughness reinforcing effect of enhancing.
Summary of the invention
The preparation method who contains modified oxidized Graphene leather fat who the purpose of this invention is to provide a kind of excellent properties based on graphene oxide.
The technical solution adopted in the present invention is:
Contain the preparation method of modified oxidized Graphene leather fat, it is characterized in that:
Realize by following steps:
Step 1: the preparation of graphene oxide:
The vitriol oil of 50 weight parts is under agitation slowly joined in the mixture of SODIUMNITRATE of the Graphite Powder 99 of 5 weight parts and 5 weight parts, the temperature of the hierarchy of control＜20 ℃ add and mix the back at the potassium permanganate that slowly adds 18 weight parts; Reacted 30 minutes down at 50 ℃ then, slowly add the deionized water of 280 weight parts again, be warming up to 100 ℃ of reactions 4 hours; Be cooled to 70 ℃ of superoxols that drip the massfraction 30% of 20 weight parts then, react and used deionized water wash after the kind in 30 minutes, regulating pH is 7.0, obtains the graphite oxide aqueous solution with 30 fens kinds of ultrasonic dispersing;
Step 2: graphene oxide and octadecyl dimethyl-2-hydroxyethyl brometo de amonio intercalated compound preparation:
Octadecyl dimethyl-2-hydroxyethyl brometo de amonio of getting 5 weight parts is dissolved in the dehydrated alcohol of 10 weight parts after the dilution, join in graphene oxide dispersion liquid 50 weight parts, stirring at room 2 hours, using ultrasonic dispersing 0.5 hour, obtain graphene oxide and octadecyl dimethyl-direct intercalated compound of 2-hydroxyethyl brometo de amonio;
Step 3: the preparation of oleic acid poly glycol monomethyl ether ester:
25 weight part oleic acid, 30 weight part poly glycol monomethyl ethers, 1200,0.6 weight part tosic acid are mixed in the reactor dry, anhydrous, that hydathode is installed and be stirred and heated to 120 ℃, be incubated 3.5 hours, reduce to room temperature and obtain oleic acid poly glycol monomethyl ether ester;
Step 4: contain the preparation of modified oxidized Graphene leather fat:
Graphene oxide intercalated compound 40 ~ 65 weight parts, oleic acid poly glycol monomethyl ether ester 9 ~ 14 weight parts, natural fats and oils 6 ~ 11 weight parts, sulphonated oil SS8 ~ 13 weight parts, Virahol 2 ~ 4 weight parts and deionized water and stirring is even, control solid content 35%, regulating the pH value is 7.0, stirred 1 hour, ultrasonic dispersing 0.5 hour, products therefrom is for containing modified oxidized Graphene leather fat.
In the step 1, the massfraction of the vitriol oil is 98%.
In the step 1, the granularity of Graphite Powder 99 is less than 30 microns, and the massfraction of carbon is 99.9%.
In the step 1, the pH regulator agent is that massfraction is 30% sodium hydroxide solution.
In the step 4, natural fats and oils is rape oil, soya-bean oil or peanut oil.
In the step 4, the pH regulator agent is that massfraction is 30% sodium hydroxide solution.
The present invention has the following advantages:
A kind of preparation method who contains the leather fat of graphene oxide of the present invention, prepared fatting agent has extraordinary bating effect for leather fiber, have the toughness reinforcing effect of enhancing simultaneously, significantly improved the Color of leather, specific absorption is very high.
Description of drawings
Fig. 1 is the signal of graphene oxide intercalated compound preparation principle.
Embodiment
The present invention will be described in detail below in conjunction with embodiment.
The crucial part of the present invention's preparation is to make graphene oxide to reach the nano level dispersion in product, has only nano level to disperse just can demonstrate effect and the effect that strengthens toughness reinforcing and softening fibre.
The preparation method who contains modified oxidized Graphene leather fat of the present invention, realized by following steps:
Step 1: the preparation of graphene oxide:
The vitriol oil of 50 weight parts is under agitation slowly joined in the mixture of SODIUMNITRATE that 5 weight parts, granularity are 99.9% Graphite Powder 99 and 5 weight parts less than 30 microns, the massfraction of carbon, the temperature of the hierarchy of control＜20 ℃ add and mix the back at the potassium permanganate that slowly adds 18 weight parts; Reacted 30 minutes down at 50 ℃ then, slowly add the deionized water of 280 weight parts again, be warming up to 100 ℃ of reactions 4 hours; Be cooled to 70 ℃ of superoxols that drip the massfraction 30% of 20 weight parts then, react and used deionized water wash after the kind in 30 minutes, regulating pH is 7.0, obtains the graphite oxide aqueous solution with 30 fens kinds of ultrasonic dispersing;
Step 2: graphene oxide and octadecyl dimethyl-2-hydroxyethyl brometo de amonio intercalated compound preparation:
Octadecyl dimethyl-2-hydroxyethyl brometo de amonio of getting 5 weight parts is dissolved in the dehydrated alcohol of 10 weight parts after the dilution, join in graphene oxide dispersion liquid 50 weight parts, stirring at room 2 hours, using ultrasonic dispersing 0.5 hour, obtain graphene oxide and octadecyl dimethyl-direct intercalated compound of 2-hydroxyethyl brometo de amonio;
Step 3: the preparation of oleic acid poly glycol monomethyl ether ester:
25 weight part oleic acid, 30 weight part poly glycol monomethyl ethers, 1200,0.6 weight part tosic acid are mixed in the reactor dry, anhydrous, that hydathode is installed and be stirred and heated to 120 ℃, be incubated 3.5 hours, reduce to room temperature and obtain oleic acid poly glycol monomethyl ether ester;
Step 4: contain the preparation of modified oxidized Graphene leather fat:
Graphene oxide intercalated compound 40 ~ 65 weight parts, oleic acid poly glycol monomethyl ether ester 9 ~ 14 weight parts, natural fats and oils 6 ~ 11 weight parts, sulphonated oil SS8 ~ 13 weight parts, Virahol 2 ~ 4 weight parts and deionized water and stirring is even, control solid content 35%, regulating the pH value is 7.0, stirred 1 hour, ultrasonic dispersing 0.5 hour, products therefrom is for containing modified oxidized Graphene leather fat.
It is 98% the vitriol oil that the vitriol oil refers in particular to massfraction.The pH regulator agent is that massfraction is 30% sodium hydroxide solution.Natural fats and oils is rape oil, soya-bean oil or peanut oil.
Embodiment one:
Step 1: the preparation of graphene oxide:
The vitriol oil of 50 weight parts is under agitation slowly joined in the mixture of SODIUMNITRATE that 5 weight parts, granularity are 99.9% Graphite Powder 99 and 5 weight parts less than 30 microns, the massfraction of carbon, the temperature of the hierarchy of control＜20 ℃ add and mix the back at the potassium permanganate that slowly adds 18 weight parts; Reacted 30 minutes down at 50 ℃ then, slowly add the deionized water of 280 weight parts again, be warming up to 100 ℃ of reactions 4 hours; Be cooled to 70 ℃ of superoxols that drip the massfraction 30% of 20 weight parts then, react and used deionized water wash after the kind in 30 minutes, regulating pH is 7.0, obtains the graphite oxide aqueous solution with 30 fens kinds of ultrasonic dispersing;
Step 2: graphene oxide and octadecyl dimethyl-2-hydroxyethyl brometo de amonio intercalated compound preparation:
Octadecyl dimethyl-2-hydroxyethyl brometo de amonio of getting 5 weight parts is dissolved in the dehydrated alcohol of 10 weight parts after the dilution, join in graphene oxide dispersion liquid 50 weight parts, stirring at room 2 hours, using ultrasonic dispersing 0.5 hour, obtain graphene oxide and octadecyl dimethyl-direct intercalated compound of 2-hydroxyethyl brometo de amonio;
Step 3: the preparation of oleic acid poly glycol monomethyl ether ester:
25 weight part oleic acid, 30 weight part poly glycol monomethyl ethers, 1200,0.6 weight part tosic acid are mixed in the reactor dry, anhydrous, that hydathode is installed and be stirred and heated to 120 ℃, be incubated 3.5 hours, reduce to room temperature and obtain oleic acid poly glycol monomethyl ether ester;
Step 4: contain the preparation of modified oxidized Graphene leather fat:
Graphene oxide intercalated compound 40 weight parts, oleic acid poly glycol monomethyl ether ester 9 weight parts, natural fats and oils rape oil 6 weight parts, sulphonated oil SS8 weight part, Virahol 2 weight parts and deionized water and stirring is even, control solid content 35%, regulating the pH value is 7.0, stirred 1 hour, ultrasonic dispersing 0.5 hour, products therefrom is for containing modified oxidized Graphene leather fat.
Embodiment two:
Step 1: the preparation of graphene oxide:
The vitriol oil of 50 weight parts is under agitation slowly joined in the mixture of SODIUMNITRATE that 5 weight parts, granularity are 99.9% Graphite Powder 99 and 5 weight parts less than 30 microns, the massfraction of carbon, the temperature of the hierarchy of control＜20 ℃ add and mix the back at the potassium permanganate that slowly adds 18 weight parts; Reacted 30 minutes down at 50 ℃ then, slowly add the deionized water of 280 weight parts again, be warming up to 100 ℃ of reactions 4 hours; Be cooled to 70 ℃ of superoxols that drip the massfraction 30% of 20 weight parts then, react and used deionized water wash after the kind in 30 minutes, regulating pH is 7.0, obtains the graphite oxide aqueous solution with 30 fens kinds of ultrasonic dispersing;
Step 2: graphene oxide and octadecyl dimethyl-2-hydroxyethyl brometo de amonio intercalated compound preparation:
Octadecyl dimethyl-2-hydroxyethyl brometo de amonio of getting 5 weight parts is dissolved in the dehydrated alcohol of 10 weight parts after the dilution, join in graphene oxide dispersion liquid 50 weight parts, stirring at room 2 hours, using ultrasonic dispersing 0.5 hour, obtain graphene oxide and octadecyl dimethyl-direct intercalated compound of 2-hydroxyethyl brometo de amonio;
Step 3: the preparation of oleic acid poly glycol monomethyl ether ester:
25 weight part oleic acid, 30 weight part poly glycol monomethyl ethers, 1200,0.6 weight part tosic acid are mixed in the reactor dry, anhydrous, that hydathode is installed and be stirred and heated to 120 ℃, be incubated 3.5 hours, reduce to room temperature and obtain oleic acid poly glycol monomethyl ether ester;
Step 4: contain the preparation of modified oxidized Graphene leather fat:
Graphene oxide intercalated compound 55 weight parts, oleic acid poly glycol monomethyl ether ester 11 weight parts, natural fats and oils soya-bean oil 8 weight parts, sulphonated oil SS10 weight part, Virahol 3 weight parts and deionized water and stirring is even, control solid content 35%, regulating the pH value is 7.0, stirred 1 hour, ultrasonic dispersing 0.5 hour, products therefrom is for containing modified oxidized Graphene leather fat.
Embodiment three:
Step 1: the preparation of graphene oxide:
The vitriol oil of 50 weight parts is under agitation slowly joined in the mixture of SODIUMNITRATE that 5 weight parts, granularity are 99.9% Graphite Powder 99 and 5 weight parts less than 30 microns, the massfraction of carbon, the temperature of the hierarchy of control＜20 ℃ add and mix the back at the potassium permanganate that slowly adds 18 weight parts; Reacted 30 minutes down at 50 ℃ then, slowly add the deionized water of 280 weight parts again, be warming up to 100 ℃ of reactions 4 hours; Be cooled to 70 ℃ of superoxols that drip the massfraction 30% of 20 weight parts then, react and used deionized water wash after the kind in 30 minutes, regulating pH is 7.0, obtains the graphite oxide aqueous solution with 30 fens kinds of ultrasonic dispersing;
Step 2: graphene oxide and octadecyl dimethyl-2-hydroxyethyl brometo de amonio intercalated compound preparation:
Octadecyl dimethyl-2-hydroxyethyl brometo de amonio of getting 5 weight parts is dissolved in the dehydrated alcohol of 10 weight parts after the dilution, join in graphene oxide dispersion liquid 50 weight parts, stirring at room 2 hours, using ultrasonic dispersing 0.5 hour, obtain graphene oxide and octadecyl dimethyl-direct intercalated compound of 2-hydroxyethyl brometo de amonio;
Step 3: the preparation of oleic acid poly glycol monomethyl ether ester:
25 weight part oleic acid, 30 weight part poly glycol monomethyl ethers, 1200,0.6 weight part tosic acid are mixed in the reactor dry, anhydrous, that hydathode is installed and be stirred and heated to 120 ℃, be incubated 3.5 hours, reduce to room temperature and obtain oleic acid poly glycol monomethyl ether ester;
Step 4: contain the preparation of modified oxidized Graphene leather fat:
Graphene oxide intercalated compound 65 weight parts, oleic acid poly glycol monomethyl ether ester 14 weight parts, natural fats and oils peanut oil 11 weight parts, sulphonated oil SS13 weight part, Virahol 4 weight parts and deionized water and stirring is even, control solid content 35%, regulating the pH value is 7.0, stirred 1 hour, ultrasonic dispersing 0.5 hour, products therefrom is for containing modified oxidized Graphene leather fat.
The experiment comparing result:
Experiment condition: goat clothes chrome tanned leather, carry out stuffing, stain test according to common process, mechanical property is according to country and the industry standard detection of taking a sample.Fatting agent adopts and contains contrasting of graphene oxide and oxygen-free Graphene, and add-on is 10% of a tare weight, and dyestuff is selected black dyes for use.The performance index of fatting agent and stuffing effect see Table 1 and table 2 respectively.The stuffing effect that contains the fatting agent of graphene oxide as can be seen from the results is better than the fatting agent of oxygen-free Graphene.
The modified oxidized Graphene leather fat of table 1 performance index
The application result of the modified oxidized Graphene leather fat of table 2
Claims (6)
1. contain the preparation method of modified oxidized Graphene leather fat, it is characterized in that:
Realize by following steps:
Step 1: the preparation of graphene oxide:
The vitriol oil of 50 weight parts is under agitation slowly joined in the mixture of SODIUMNITRATE of the Graphite Powder 99 of 5 weight parts and 5 weight parts, the temperature of the hierarchy of control＜20 ℃ add the potassium permanganate that slowly adds 18 weight parts after mixing again; Reacted 30 minutes down at 50 ℃ then, slowly add the deionized water of 280 weight parts again, be warming up to 100 ℃ of reactions 4 hours; Be cooled to 70 ℃ of superoxols that drip the massfraction 30% of 20 weight parts then, react and used deionized water wash after the kind in 30 minutes, regulating pH is 7.0, obtains the graphite oxide aqueous solution with 30 fens kinds of ultrasonic dispersing;
Step 2: graphene oxide and octadecyl dimethyl-2-hydroxyethyl brometo de amonio intercalated compound preparation:
Octadecyl dimethyl-2-hydroxyethyl brometo de amonio of getting 5 weight parts is dissolved in the dehydrated alcohol of 10 weight parts after the dilution, join in graphite oxide aqueous solution 50 weight parts, stirring at room 2 hours, use ultrasonic dispersing again 0.5 hour, and obtained graphene oxide and octadecyl dimethyl-direct intercalated compound of 2-hydroxyethyl brometo de amonio;
Step 3: the preparation of oleic acid poly glycol monomethyl ether ester:
25 weight part oleic acid, 30 weight part poly glycol monomethyl ethers, 1200,0.6 weight part tosic acid are mixed in the reactor dry, anhydrous, that hydathode is installed and be stirred and heated to 120 ℃, be incubated 3.5 hours, reduce to room temperature and obtain oleic acid poly glycol monomethyl ether ester;
Step 4: contain the preparation of modified oxidized Graphene leather fat:
Graphene oxide and direct intercalated compound 40 ~ 65 weight parts of octadecyl dimethyl-2-hydroxyethyl brometo de amonio, oleic acid poly glycol monomethyl ether ester 9 ~ 14 weight parts, natural fats and oils 6 ~ 11 weight parts, sulphonated oil SS8 ~ 13 weight parts, Virahol 2 ~ 4 weight parts and deionized water and stirring is even, control solid content 35%, regulating the pH value is 7.0, stirred 1 hour, ultrasonic dispersing 0.5 hour, products therefrom is for containing modified oxidized Graphene leather fat.
2. the preparation method who contains modified oxidized Graphene leather fat according to claim 1 is characterized in that:
In the step 1, the massfraction of the vitriol oil is 98%.
3. the preparation method who contains modified oxidized Graphene leather fat according to claim 1 and 2 is characterized in that:
In the step 1, the granularity of Graphite Powder 99 is less than 30 microns, and the massfraction of carbon is 99.9%.
4. the preparation method who contains modified oxidized Graphene leather fat according to claim 3 is characterized in that:
In the step 1, the pH regulator agent is that massfraction is 30% sodium hydroxide solution.
5. the preparation method who contains modified oxidized Graphene leather fat according to claim 4 is characterized in that:
In the step 4, natural fats and oils is rape oil, soya-bean oil or peanut oil.
6. the preparation method who contains modified oxidized Graphene leather fat according to claim 5 is characterized in that:
In the step 4, the pH regulator agent is that massfraction is 30% sodium hydroxide solution.
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| CN103242007B (en) * | 2013-05-22 | 2014-10-22 | 陕西科技大学 | Preparation method of graphene oxide modified polymer cement waterproof coating |
| CN104324689A (en) * | 2014-10-24 | 2015-02-04 | 陕西科技大学 | Preparation method of modified graphene oxide and method for removing bisphenol A from water |
| CN105132598B (en) * | 2015-07-29 | 2017-06-06 | 浙江理工大学 | A kind of guard method for full water leather cultural relic |
| CN107164587A (en) * | 2017-06-28 | 2017-09-15 | 常州凯恒纺织品有限公司 | A kind of leather fat |
| CN108950104B (en) * | 2018-02-08 | 2020-10-27 | 陕西科技大学 | Hyperbranched natural grease leather fatting agent containing graphene oxide and preparation method and application thereof |
| CN108998596A (en) * | 2018-09-04 | 2018-12-14 | 四川大学 | A kind of graphene-based flame-retardant leather fatting agent and preparation method thereof |
| CN113036306A (en) * | 2021-02-20 | 2021-06-25 | 山东天瀚新能源科技有限公司 | Silicon-doped lithium supplement technical scheme and assembly method of lithium ion battery |
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| DE102008040953A1 (en) * | 2008-08-01 | 2010-02-04 | Forschungsinstitut für Leder und Kunststoffbahnen gGmbH | Substance, useful for equipping e.g. leather and furs with fungicidal protection, comprises carboxylic acids with alkyl residue, which are saturated or mono- or polyunsaturated, branched or substituted on the alkyl chain |
| JP2010121012A (en) * | 2008-11-18 | 2010-06-03 | Midori Hokuyo Kk | Leather for instrument panel |
| CN102242229A (en) * | 2011-05-18 | 2011-11-16 | 山东力厚轻工新材料有限公司 | Modified phospholipid fat-liquoring agent and preparation method thereof |
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| SU1178769A1 (en) * | 1984-02-03 | 1985-09-15 | Институт нефтехимических процессов АН АзССР | Composition for leather fattening |
| BRPI0819700B1 (en) * | 2007-12-19 | 2019-03-26 | Stahl International B.V. | Leather Retanning and Lubricating Composition, Production Process and Use |
| CN101831513A (en) * | 2009-03-13 | 2010-09-15 | 上海喜若飞精细化工有限公司 | Greasing agent for improving strength of leather and preparation method thereof |
| CN101985517A (en) * | 2010-09-21 | 2011-03-16 | 中国科学院长春应用化学研究所 | Synthesis method of conductive polyaniline-graphene composite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008040953A1 (en) * | 2008-08-01 | 2010-02-04 | Forschungsinstitut für Leder und Kunststoffbahnen gGmbH | Substance, useful for equipping e.g. leather and furs with fungicidal protection, comprises carboxylic acids with alkyl residue, which are saturated or mono- or polyunsaturated, branched or substituted on the alkyl chain |
| JP2010121012A (en) * | 2008-11-18 | 2010-06-03 | Midori Hokuyo Kk | Leather for instrument panel |
| CN102242229A (en) * | 2011-05-18 | 2011-11-16 | 山东力厚轻工新材料有限公司 | Modified phospholipid fat-liquoring agent and preparation method thereof |
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