CN102553504A - Preparation method of emulsion, leather care emulsion, and use leather care emulsion - Google Patents
Preparation method of emulsion, leather care emulsion, and use leather care emulsion Download PDFInfo
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- CN102553504A CN102553504A CN2012100162045A CN201210016204A CN102553504A CN 102553504 A CN102553504 A CN 102553504A CN 2012100162045 A CN2012100162045 A CN 2012100162045A CN 201210016204 A CN201210016204 A CN 201210016204A CN 102553504 A CN102553504 A CN 102553504A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00889—Mixing
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Abstract
The invention relates to a preparation method of emulsion, a leather care emulsion and use of the leather care emulsion. On the one hand, the invention relates to the preparation method of the emulsion, comprising the step of: treating aqueous components and hydrophobic components in a microreactor system, to obtain the emulsion. The invention further relates to the leather care emulsion, comprising: (i) the emulsion obtained according to the method provided by the invention; and (ii) the other leather finshing assistant agents selecting from polyurethane emulsion. The invention further relates to the use of the leather care emulsion in coating or caring a leather product. The method can be used for preparing cation wax emulsion by a microreactor technology, and preparing the product which is stable and good in performance by a small quantity of emulsifying agent and assistant agent.
Description
Technical field
The present invention relates to a kind of emulsion preparation method and leather nursing emulsion, its purposes, relate in particular to cationic wax emulsion preparation method and leather nursing emulsion, its purposes.
Background technology
Cationic wax emulsion is a kind of covering with paint auxiliary agent that can apply in the leather processing, and it is better than the emulsion spreadability of anionic and nonionic, and film forming is even.
At present mainly be in agitated reactor, to prepare cationic wax emulsion with mechanical agitation at a high speed.But cationic wax emulsion has poor stability, very easily the shortcoming of layering.Therefore, just need to add more surfactant (emulsifying agent) and auxiliary agent in order to prepare stable good product emulsion, and can cause in preparation that so a large amount of bubbles is unfavorable for production and processing, also increased production cost simultaneously.
Adopt traditional approach to prepare paraffin wax emulsions, have to add more emulsifying agent for the stability of product emulsion.And the hydrophily of emulsifying agent is stronger, can make the moisture-proof sassafras property of covering with paint, lacquer, colour wash, etc. auxiliary agent relatively poor.Therefore, how to reduce the emulsifying agent in the leather finish auxiliary agent consumption, improve to cover with paint, lacquer, colour wash, etc. performance and become a problem demanding prompt solution.
The modular microfluidic reaction technology is for developing new reaction process, setting up the brand-new road that open up in the chemical plant have economic benefit.Its outstanding part be its can realize that high-speed mixing, efficient heat transfer, the narrow distribution of reactant residence time, system responses are convenient to rapidly to control and online chemical volume seldom, thereby can obtain higher safe performance.
But do not adopt little reaction technology to prepare the report of emulsion in the prior art.
Summary of the invention
The present invention relates to a kind of method for preparing emulsion, comprising: water composition and hydrophobicity composition are handled in the microreactor system, obtained emulsion.
Preferably, emulsion comprises: (A) hydrophobicity composition; (B) water; And optional (C) emulsifying agent.
Preferably, water composition is the aqueous solution that contains emulsifying agent.
Preferably, the hydrophobicity composition is selected from wax, oil, fat, higher alcohols and composition thereof.
Preferably, the hydrophobicity composition is selected from wax, higher alcohols and composition thereof.
Preferably, the hydrophobicity composition comprises wax and higher alcohols.
Preferably, wax is selected from biological wax, mineral wax, synthetic wax and composition thereof.
Preferably, wax is selected from paraffin, beeswax, palm wax, spermaceti, ant wax, lanocerin, haze tallow, flax wax, Chinese insect wax, candelila wax, Ka Naba wax, Japan tallow, ore deposit ceresine, ceresine, montanin wax, brown alabaster wax, pertroleum wax, microwax, Fischer-Tropsch wax, Tissuemat E, polypropylene wax, the existing property wax of chemistry, chlorinated paraffin wax, emulsifying wax and composition thereof.
Preferably, higher alcohols are C
6～C
24Alkylol.
Preferably, higher alcohols are selected from: hexanol such as n-hexyl alcohol, enanthol such as n-heptanol, octanol such as n-octyl alcohol, nonyl alcohol such as n-nonyl alcohol, decyl alcohol such as Decanol, undecylenic alcohol such as positive undecylenic alcohol, 12 carbon alcohol as positive 12 carbon alcohol, 13 carbon alcohol as positive 13 carbon alcohol, ten four carbon alcohols such as positive ten four carbon alcohols, pentadecanol such as positive pentadecanol, 16 carbon alcohol as positive 16 carbon alcohol, 17 carbon alcohol as positive 17 carbon alcohol, octadecanol such as positive octadecanol, 19 carbon alcohol as positive 19 carbon alcohol, eicosanol such as positive eicosanol, two undecylenic alcohols such as positive two undecylenic alcohols, 22 carbon alcohol as positive 22 carbon alcohol, 23 carbon alcohol as positive 23 carbon alcohol, tetracosa carbon is pure as positive tetracosa carbon alcohol and composition thereof.
Preferably, the hydrophobicity composition comprises grease.
Preferably, emulsifying agent is selected from cationic surfactant, anion surfactant, amphoteric surfactant, non-ionic surface active agent and composition thereof.
Preferably, emulsifying agent is selected from cationic surfactant, non-ionic surface active agent and composition thereof.
Preferably, emulsifier package cation surfactant and non-ionic surface active agent perhaps are made up of cationic surfactant and non-ionic surface active agent.
Preferably, cationic surfactant is selected from one or more in amine salt cationic surfactant, the quaternary cationics.
Preferably, cationic surfactant is selected from: kation alkyl polysaccharide glycosides, hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride, lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride, imidazoline quaternary ammonium salt, hexadecanol polyoxyethylene ether trimethyl ammonium chloride, polyoxyethylene octadecanol base trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride and composition thereof.
Preferably, non-surface-active agent is selected from one or more in polyoxyethylene alkane ether, polyoxyethylene fatty acid glyceride, glycol fatty acid ester and the polyoxyethylene fatty acid amine.
Preferably; Non-ionic surface active agent is selected from: sorbitan monolaurate, polyoxyethylene 20 sorbitan monolaurate AEO, polyoxyethylene alkane ether, polyoxyethylene fatty acid glyceride, glycol fatty acid ester, polyoxyethylene fatty acid amine, and composition thereof.
Preferably, based on the emulsion gross weight, the emulsifying agent consumption is≤11%.
Preferably, based on the emulsion gross weight, the emulsifying agent consumption is 5%～10%.
Preferably, based on the emulsion gross weight, solid content is 25%～50%.
Preferably, wherein, based on the emulsion gross weight, cationic surfactant concentration is 1%～10%.
Preferably, based on the emulsion gross weight, non-ionic surfactant concentration is 0.5%～5%.
Preferably, based on the emulsion gross weight, higher alcohols content is 0.5%～5%.
Preferably, based on the emulsion gross weight, solid content is 25%～50%.
Preferably, based on the emulsion gross weight, solid content is 30%～35%.
Preferably, method of the present invention comprises:
(a) with water composition and the preheating of hydrophobicity composition;
(b) water composition and hydrophobicity composition are handled in the microreactor system, obtained emulsion.
Preferably, in step (a), preheat temperature is to be enough to temperature that all the components is in a liquid state.
Preferably, preheat temperature is 60～100 ℃.
Preferably, the microreactor system comprises reactor, and wherein temperature of reactor is more than or equal to preheat temperature.
The invention still further relates to the emulsion that obtains according to the method for the invention.
The invention still further relates to a kind of leather nursing emulsion, comprise:
(i) emulsion that obtains according to the method for the invention;
(ii) other leather finish auxiliary agents.
Preferably, other leather finish auxiliary agents are selected from one or more in polyaminoester emulsion, polyacrylic acid emulsion, the nitrocotton emulsion.
The invention still further relates to this leather nursing emulsion and applying or nursing the purposes in the leather and fur products.
The present invention provides a kind of especially new technology of cationic wax emulsion of emulsion for preparing, and the present invention can economize in raw materials, and is simple to operate, good product quality.
The present invention selects microreactor technology preparation cationic wax emulsion for use, has prepared stable and the good product of performance with a spot of emulsifying agent and auxiliary agent.
Description of drawings
Fig. 1 is the sketch map of microreactor used in the present invention system.
The specific embodiment
In the present invention, under the situation of not contradiction or conflict, all embodiment of the present invention, embodiment and characteristic can make up each other.
In the present invention, unit, parts, reagent etc. both can be purchased, also can be according to content self-control disclosed by the invention.
In the present invention, for outstanding emphasis of the present invention, the omission that some conventional operations and unit, parts are carried out, or only do simple description.
Except that other statement, all concentration, content, proportioning, the ratios of the present invention all are by weight.
The inventor unexpectedly finds, adopts microreactor to prepare the consumption that emulsion (particularly paraffin wax emulsions) can significantly reduce emulsifying agent, and prepared emulsion (particularly paraffin wax emulsions) has excellent stability simultaneously.Adopt the emulsion (particularly paraffin wax emulsions) of method preparation of the present invention to handle leather, its water-tolerant, wet-rub resistance with excellence, softness improves, and permeability is good, and outward appearance is good.
One aspect of the present invention relates to a kind of method for preparing emulsion, comprising: water composition and hydrophobicity composition are handled in the microreactor system, obtained emulsion.
Preferably, water composition and hydrophobicity composition are handled with liquid state in the microreactor system, obtained emulsion.
Preferably, the present invention's method of preparing emulsion comprises:
(a) with water composition and the preheating of hydrophobicity composition;
(b) water composition and hydrophobicity composition are handled in the microreactor system, obtained emulsion.
When comprising under the normal temperature for solid-state composition in the emulsion, when especially the hydrophobicity composition was wax, method of the present invention comprised (a) preheating step.
Preheat temperature is to be enough to temperature that all the components is in a liquid state.Preferably, in step (a), preheat temperature is 60～100 ℃, preferred 70～100 ℃, and most preferably 80～90 ℃.
Preferably, the microreactor system comprises reactor.Preferably, temperature of reactor is to be enough to temperature that all the components is in a liquid state.Preferably, temperature of reactor is preferably greater than preheat temperature more than or equal to preheat temperature.Preferably, temperature of reactor is 70～120 ℃, preferred 70～110 ℃, and most preferably 80～100 ℃.
Emulsion of the present invention comprises: (A) hydrophobicity composition; (B) water; And optional (C) emulsifying agent.
Preferably, emulsion of the present invention comprises: (A) hydrophobicity composition; (B) water; And (C) emulsifying agent.
Preferably, water composition is the aqueous solution, preferably contains the aqueous solution of emulsifying agent.In another embodiment, do not comprise emulsifying agent in the emulsion.
(A) hydrophobicity composition
The hydrophobicity composition also can be called oiliness composition or oiliness material.
Preferably, the hydrophobicity composition is selected from wax, oil, fat, higher alcohols and composition thereof, preferred wax, higher alcohols and composition thereof.A kind of preferred embodiment in, the hydrophobicity composition comprises wax and higher alcohols.
Preferably, wax is selected from biological wax, mineral wax, synthetic wax and composition thereof.
Preferably, wax is selected from paraffin, beeswax, palm wax, spermaceti, ant wax, lanocerin, haze tallow, flax wax, Chinese insect wax (chinese insect wax), candelila wax (candelilla wax), Ka Naba wax (carnauba wax), Japan tallow, ore deposit ceresine (oecerite), ceresine (ceresin), montanin wax (montan wax), brown alabaster wax (lignite parffin wax), pertroleum wax (petroleum wax), microwax (microcrystalline waxes), Fischer-Tropsch wax (Fiseher-Tropsch wax), Tissuemat E (polyethylene waxes), polypropylene wax (polypropylene waxes), the existing property wax (chemical derivatives of existing waxes) of chemistry, chlorinated paraffin wax (chlorinated paraffin wax), emulsifying wax (emulsifiable wax) and composition thereof.
Preferably, higher alcohols are C
6～C
24Alkylol, preferred C
8～C
24Alkylol, more preferably C
10～C
24Alkylol, most preferably C
12～C
20Alkylol.
Preferably, higher alcohols are selected from: hexanol such as n-hexyl alcohol, enanthol such as n-heptanol, octanol such as n-octyl alcohol, nonyl alcohol such as n-nonyl alcohol, decyl alcohol such as Decanol, undecylenic alcohol such as positive undecylenic alcohol, 12 carbon alcohol as positive 12 carbon alcohol, 13 carbon alcohol as positive 13 carbon alcohol, ten four carbon alcohols such as positive ten four carbon alcohols, pentadecanol such as positive pentadecanol, 16 carbon alcohol as positive 16 carbon alcohol, 17 carbon alcohol as positive 17 carbon alcohol, octadecanol such as positive octadecanol, 19 carbon alcohol as positive 19 carbon alcohol, eicosanol such as positive eicosanol, two undecylenic alcohols such as positive two undecylenic alcohols, 22 carbon alcohol as positive 22 carbon alcohol, 23 carbon alcohol as positive 23 carbon alcohol, tetracosa carbon is pure as positive tetracosa carbon alcohol and composition thereof.
Preferably, the hydrophobicity composition comprises grease.Preferably, grease is selected from fat like natural fat, oily like fat oil, wax, resin and derivative thereof and/or petroleum distillate and downstream product thereof.
For example, fatty material comprises plant and animal fat and oily, and for example iodine number is the plant and animal fat of 10-200 and oily.
Preferably, fatty material is selected from butter, animal oil, neat's foot oil, lard, rapeseed oil, olive oil, nut oil and castor oil.
(C) emulsifying agent
Preferably, emulsifying agent is a surfactant.Preferably, emulsifying agent is selected from cationic surfactant, anion surfactant, amphoteric surfactant, non-ionic surface active agent and composition thereof, and preferred emulsifier is selected from cationic surfactant, non-ionic surface active agent and composition thereof.
A kind of preferred embodiment in, emulsifier package cation surfactant and non-ionic surface active agent perhaps are made up of cationic surfactant and non-ionic surface active agent.
A kind of preferred embodiment in, emulsion of the present invention does not comprise anion surfactant.A kind of preferred embodiment in, emulsion of the present invention does not comprise amphoteric surfactant.
As surfactant, that can enumerate has, for example, and anion surfactants such as carboxylate, sulfonate, sulfuric acid, phosphate ester salt; Cationic surfactant such as amine salt, quaternary ammonium salt; Amphoteric surfactantes such as carboxybetaine, aminocarboxylate, imidazolinium betaine; Non-surface-active agents such as polyoxyethylene alkane ether, polyoxyethylene fatty acid glyceride, glycol fatty acid ester, polyoxyethylene fatty acid amine etc.
Amine salt is selected from fatty amine salt, ethanolamine salt and polyethylene polyamines salt.For example, fatty amine salt is with in hydrochloric acid, formic acid, the acetate and the product that obtains of kiber alkyl amine, secondary amine and tertiary amine.For example, ethanolamine salt is the product of acid and one, two, triethanolamine reaction.For example, polyethylene polyamines salt is that alkyl halide can obtain different N-alkyl polyamines with Diethylenetriamine, the reaction of three second tetramines.
Quaternary ammonium salt is generally made by tertiary amine and hydrocarbylation reagent reactings such as alcohol, halogenated hydrocarbons, dimethyl suflfate.
For example, the quaternary ammonium salt cationic surfactant general formula does
[NRR
1R
2R
3]
+X
-
Wherein,
R is C10～C18 alkyl,
R
1, R
2, R
3Identical or different, be independently selected from C1～C5 alkyl, for example methyl, ethyl or propyl group, perhaps R
1, R
2, R
3In one be C10～C18 alkyl or C6-C20 aryl, benzyl for example, other are independently selected from C1～C5 alkyl;
X is an anionic group, preferred chlorine, bromine, iodine, more preferably chlorine or bromine.
Preferably, cationic surfactant is selected from: kation alkyl polysaccharide glycosides, hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride, lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride, imidazoline quaternary ammonium salt, hexadecanol polyoxyethylene ether trimethyl ammonium chloride (1631), polyoxyethylene octadecanol base trimethyl ammonium chloride (1831), dodecyl benzyl dimethyl ammonium chloride (1227) and composition thereof.
Preferably; Non-ionic surface active agent is selected from: sorbitan monolaurate (for example Span 20, and Span 60), polyoxyethylene 20 sorbitan monolaurate (for example polysorbas20, Tween 80), AEO, polyoxyethylene alkane ether, polyoxyethylene fatty acid glyceride, glycol fatty acid ester, polyoxyethylene fatty acid amine and composition thereof.
Preferably, amphoteric surfactant is selected from: carboxybetaine, sulfobetaines, aminocarboxylate, imidazolinium betaine, phosphoric acid fat betaine, amine oxide and composition thereof.
Preferably, based on the emulsion gross weight, emulsifying agent consumption≤15%, preferred≤10%, more preferably≤9%, further preferably≤6%, most preferably≤4%.
Preferably, based on the emulsion gross weight, emulsifying agent consumption >=0.01%, preferred >=0.1%, more preferably >=0.5%, further preferably >=0.8%, especially preferably >=1%, most preferably >=2%.
Preferably, based on the emulsion gross weight, the emulsifying agent consumption is 0.1%～15%, and is preferred 1%～15%, more preferably 2%～15%, and further preferred 2%～10%, preferred especially 2%～9%, most preferably >=2%～6%.
Preferably, based on the emulsion gross weight, the emulsifying agent consumption is≤11%, preferred≤10%, more preferably≤9%, further preferably≤8%, most preferably≤6%.
Preferably, based on the emulsion gross weight, the emulsifying agent consumption is 5%～10%, and is preferred 5%～9%, more preferably 5%～8%, most preferably 5%～6%.
Preferably, based on the emulsion gross weight, solid content >=25%, preferred >=30%, more preferably >=35%.
Preferably, based on the emulsion gross weight, solid content is 25%～50%, and is preferred 30%～50%, more preferably 30%～45%, further preferred 30%～40%, preferred especially 30%～35%.
Preferably, based on the emulsion gross weight, wax content >=20%, preferred >=25%, more preferably >=30%.
Preferably, based on the emulsion gross weight, wax content is 15%～40%, and is preferred 20%～40%, more preferably 25%～40%.
Preferably, based on the emulsion gross weight, cationic surfactant concentration is 1%～10%, and is preferred 2%～8%, more preferably 2%～5%.
Preferably, based on the emulsion gross weight, non-ionic surfactant concentration is 0.5%～5%, and is preferred 1%～5%, more preferably 1%～2%.
Preferably, based on the emulsion gross weight, higher alcohols content is 0.5%～5%, and is preferred 1%～5%, more preferably 1%～4%, most preferably 1%～3.5%.
A kind of preferred embodiment in, emulsion of the present invention comprises or is made up of following component: wax; Cationic surfactant; Non-ionic surface active agent; Higher alcohols; The water of surplus.
A kind of preferred embodiment in, emulsion of the present invention comprises or is made up of following component: paraffin; Beeswax; Palm wax; Cationic surfactant; Non-ionic surface active agent; Higher alcohols; The water of surplus.
A kind of preferred embodiment in, emulsion of the present invention comprises or is made up of following component:
Wax 15%～40%, preferred 20%～40%, more preferably 25%～40%;
Cationic surfactant 1%～10%, preferred 2%～8%, more preferably 2%～5%;
Non-ionic surface active agent 0.5%～5%, preferred 1%～5%, more preferably 1%～2%;
Higher alcohols 0.5%～5%, preferred 1%～5%, more preferably 1%～4%;
The water of surplus.
A kind of preferred embodiment in, emulsion of the present invention comprises or is made up of following component:
Wax 15%～40%, preferred 20%～40%, more preferably 25%～40%;
Cationic surfactant 1%～10%, preferred 2%～8%, more preferably 2%～5%;
Non-ionic surface active agent 0.5%～5%, preferred 1%～5%, more preferably 1%～2%;
Higher alcohols 0.5%～5%, preferred 1%～5%, more preferably 1%～4%;
Water 50%～70%.
A kind of preferred embodiment in, emulsion of the present invention comprises or is made up of following component:
Cationic surfactant 1%～10%, preferred 2%～8%, more preferably 2%～5%;
Non-ionic surface active agent 0.5%～5%, preferred 1%～5%, more preferably 1%～2%;
Higher alcohols 0.5%～5%, preferred 1%～5%, more preferably 1%～4%;
The water of surplus.
A kind of preferred embodiment in, emulsion of the present invention comprises or is made up of following component:
Cationic surfactant 1%～10%, preferred 2%～8%, more preferably 2%～5%;
Non-ionic surface active agent 0.5%～5%, preferred 1%～5%, more preferably 1%～2%;
Higher alcohols 0.5%～5%, preferred 1%～5%, more preferably 1%～4%;
Water 50%～70%.
During preparation, emulsifying agent is soluble in water, stir.The wax and the aqueous solution are preheated to 80 ℃ respectively, get into the microreactor system then and are mixed with.
The module of microreactor used in the present invention system is as shown in Figure 1.The microreactor system comprises and imports and exports module 1, heat exchange module 2, adiabatic module 3, blender 4, reactor 5, temperature probe 6.Heat exchange module 2 is used for charging is heated, and discharging is cooled off.
Importing and exporting the no pipe that module 1 is used between the module of microreactor system connects.Reaction mass gets into microreactor from external container, need be by conduit and standard connector.Different except the sign of sign fluid flow direction, import identical (1a: water inlet with the derivation Module Design; 1b: hydrophobic inlet mutually; 1c: the emulsion outlet).
Adiabatic module 3: the temperature difference is bigger between two modules of required connection, and when only allowing to have between two modules very little heat conduction, can adopt adiabatic link block 3.
Stacked blender 4 utilizes the operation principle convection cell of cutting apart repeatedly with merging to mix.Briefly, two fluid streams are cut apart, and just form four fluid streams after remerging.After this process was carried out several again with range upon range of mode, fluid just was divided into a lot of strands of threads.Add the diffusion and the secondary flow effect that in this process, produce, just produced a kind of mixed process very fast.
Temperature probe 6 is used to measure the temperature of fluid, and is connected with computer, realizes temperature controlling through the control to computer.
A kind of preferred embodiment in; Water and wax are used 2 charge pumps respectively, are proportionally joined in the little reaction system of module by pump, and 80 ℃ of the interior oil temperature of heat exchanger are set; Temperature of reactor is set; When the temperature indicator temperature in the control module chart no longer changes, collect product, obtain cationic wax emulsion.
Preferably, the flow of pump is at 2ml/min～20ml/min, 80～100 ℃ of temperature of reactor.
Cationic emulsified wax performance indications: white emulsion, solid content 30%～35%, pH:4～6.Product stability is: under 45 ℃, and three months outward appearance no changes.
The present invention relates to the emulsion that adopts method preparation of the present invention on the other hand.
Preferably, emulsion of the present invention is the wax emulsion, preferred cationic wax emulsion.
The present invention relates to the purposes of microreactor system in the preparation emulsion on the other hand.
The present invention relates to a kind of leather nursing emulsion or leather finish emulsion on the other hand, comprises:
(i) emulsion that obtains according to the method for the invention;
(ii) other leather finish auxiliary agents.
Preferably, the covering with paint auxiliary agent is selected from one or more in polyaminoester emulsion, polyacrylic acid emulsion, the nitrocotton emulsion.
The present invention relates to leather nursing emulsion of the present invention or the purposes of leather finish emulsion in the coating leather goods on the other hand.
The present invention relates to leather nursing emulsion of the present invention or the purposes of leather finish emulsion in the nursing leather and fur products on the other hand.
Microreactor technology has following advantage in application:
(I) the size advantage that reduces to bring
1. linear dimension reduces: along with reducing of linear dimension, the gradient of some physical quantitys increases very soon, for example thermograde; Barometric gradient; Concentration gradient and density gradient etc. cause mass transfer, driving force of heat transfer to increase, thereby have enlarged the diffusion flux of unit volume or area.Increase greatly like heat transfer coefficient.
2. the increase of area-volume ratio: the increase of specific area also can be strengthened course of reaction except can augmentation of heat transfer
3. volume reduces: owing to reducing of linear dimension, the volume of microreactor sharply reduces, even may diminish to several microlitres.When a large-scale batch process is replaced with continuous micromodule equipment, this difference is just more obvious.Reaction time shortens greatly, and has improved the selectivity of the security course of reaction of equipment greatly.
(II) advantage brought of modularization increase
1. important feature of microreactor (system) is that its basic module can be operated in parallel; Be that material passes through in the passage that the common feed pipeline gets into a plurality of micro-structural modules respectively; Therefore the disposal ability of microreactor can improve through the number that increases functional module; Conventional reactors then need realize through amplifying consersion unit step by step, so improved the flexibility of producing greatly.
2. owing to this modular system, can dismantle very easily soon very much and assemble, thus can be according to the collocation of technology adjusting module, the screening and the optimization technology that make experiment or produce fast and low-cost.
(III) be applied in the preparation cationic wax emulsion, the reaction time is short, and the raw material consumption is few, good product quality.Play the effect of practicing thrift cost.
(1) high efficient mixed
Microchannel size in the microreactor system, mixes to the submillimeter order of magnitude in sub-micron, and the emulsion particle of formation is little, and emulsion system is stable;
(2) efficient heat transfer
Because the passage of microreactor system is very little, through heat exchange module the time, solution is divided into the quite little sub-fluid of many bulks, and the Reynolds number of this a little fluid is lower, and fluid shows as laminar flow more, and heat-transfer effect is good;
(3) efficient control
The reactant of microreactor system has charge pump to squeeze into reaction system, and passage is little, and fluid rate difference is little;
(4) continuity
Can successive reaction with the microreactor system, and the temperature, pressure of whole system controlled by computer, thus obtain more stabilized products.
Without being limited by theory, it is believed that the emulsion that the microreactor mode prepares, owing to be the emulsion that oil phase and water prepare under the high velocity impact situation; Its emulsion particle is very little, except helping emulsion-stabilizing, because its particle is little; Part oil, wax infiltrate intracutaneous portion more easily, make leather soft more.Owing to its emulsion-stabilizing, can reduce the emulsifying agent consumption of about 20-30% in operation, reduce cost on the one hand, the more important thing is the many physical properties such as the softness that have increased leather, moisture-proof is wiped, permeability.
The present invention selects microreactor technology preparation cationic wax emulsion for use, has prepared stable and the good product of performance with a spot of emulsifying agent and auxiliary agent.
Embodiment
(I) reagent and equipment
(A) hydrophobicity composition
(A1) wax
(a11) paraffin is available from China PetroChemical Corporation;
(a12) beeswax is available from Dongguang, Hebei company;
(a13) palm wax is available from FONCEPI company (Brazil);
(A2) higher alcohols
(a21) hexadecanol is available from Wuxi Dong Tai chemical company;
(a22) 18 alcohol are available from Wuxi Dong Tai chemical company;
(C) emulsifying agent
(C1) cationic surfactant
(c11) kation alkyl polysaccharide glycosides is available from Henan provincial highway purifying worker technology Co., Ltd;
(c12) hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride is available from Henan provincial highway purifying worker technology Co., Ltd;
(c13) lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride is available from Henan provincial highway purifying worker technology Co., Ltd;
(C2) non-ionic surface active agent
(c21) Span 20, available from CRODA;
(c22) Span 60, available from CRODA;
(c23) AEO is available from Luo Diya (circling in the air) company.
Microreactor system: available from Bayer-Ei Fielder Micro-Technology company.
(II) emulsion preparation
Embodiment 1
With 18g paraffin, the 4g beeswax, 4g palm wax, 1g Span 20 puts into beaker with the 1g hexadecanol, is heated to 80 ℃ of fusings, stirs.5g kation alkyl polysaccharide glycosides is dissolved in 65g water, is heated to 80 ℃.The flow that oiliness material feed pump is set is 3.5ml/min, and the flow that the aqueous materials feed pump is set is 8ml/min.It is 90 ℃ that heating heat exchange module oil bath temperature is set, and the cooling heat transferring module is led to condensed water.Reactor module heating oil bath is set to 90 ℃.When equitemperature rises to design temperature, open two feed pumps simultaneously.When treating that the thermal module displays temperature arrives 80 ℃ of reaction temperatures, can collect the cationic wax emulsion finished product from outlet.
Cationic emulsified wax performance indications: white emulsion, solid content 33.7%, PH:4.5.Product stability, 45 ℃, three months outward appearance no changes.
With 14g paraffin, the 6.5g beeswax, 6.5g palm wax, 1.5g Span 60 puts into beaker with 2g 18 alcohol, is heated to 80 ℃ of fusings, stirs.8g hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride is dissolved in 70g water, is heated to 80 ℃.The flow that oiliness material feed pump is set is 5.4ml/min, and the flow that the aqueous materials feed pump is set is 12ml/min.It is 100 ℃ that heating heat exchange module oil bath temperature is set, and the cooling heat transferring module is led to condensed water.Reactor module heating oil bath is set to 100 ℃.When equitemperature rises to design temperature, open two feed pumps simultaneously.When treating that the thermal module displays temperature arrives 90 ℃ of reaction temperatures, can collect the cationic wax emulsion finished product from outlet.
Cationic emulsified wax performance indications: white emulsion, solid content 35.5%, PH:5.0.Product stability, 45 ℃, three months outward appearance no changes.
With 8g paraffin, the 8g beeswax, 8g palm wax, 2g Span 20 puts into beaker with 3.5g 18 alcohol, is heated to 80 ℃ of fusings, stirs.7.5g lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride is dissolved in 70g water, is heated to 80 ℃.The flow that oiliness material feed pump is set is 6.7ml/min, and the flow that the aqueous materials feed pump is set is 15ml/min.It is 110 ℃ that heating heat exchange module oil bath temperature is set, and the cooling heat transferring module is led to condensed water.Reactor module heating oil bath is set to 110 ℃.When equitemperature rises to design temperature, open two feed pumps simultaneously.When treating that the thermal module displays temperature arrives 100 ℃ of reaction temperatures, can collect the cationic wax emulsion finished product from outlet.
Cationic emulsified wax performance indications: white emulsion, solid content 34.6%, PH:4.7.Product stability, 45 ℃, three months outward appearance no changes.
Embodiment 4
With 10g paraffin, the 6g beeswax, 6g palm wax, 2.5g Span 60 puts into beaker with the 2g hexadecanol, is heated to 80 ℃ of fusings, stirs.6g lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride is dissolved in 65g water, is heated to 80 ℃.The flow that oiliness material feed pump is set is 5.4ml/min, and the flow that the aqueous materials feed pump is set is 12ml/min.It is 110 ℃ that heating heat exchange module oil bath temperature is set, and the cooling heat transferring module is led to condensed water.Reactor module heating oil bath is set to 110 ℃.When equitemperature rises to design temperature, open two feed pumps simultaneously.When treating that the thermal module displays temperature arrives 100 ℃ of reaction temperatures, can collect the cationic wax emulsion finished product from outlet.
Cationic emulsified wax performance indications: white emulsion, solid content 33.3%, PH:5.3.Product stability, 45 ℃, three months outward appearance no changes.
With 12g paraffin, the 5g beeswax, 5g palm wax, 2g AEO and 3g 18 alcohol are put into beaker, are heated to 80 ℃ of fusings, stir.6g hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride is dissolved in 65g water, is heated to 80 ℃.The flow that oiliness material feed pump is set is 6.7ml/min, and the flow that the aqueous materials feed pump is set is 15ml/min.It is 100 ℃ that heating heat exchange module oil bath temperature is set, and the cooling heat transferring module is led to condensed water.Reactor module heating oil bath is set to 100 ℃.When equitemperature rises to design temperature, open two feed pumps simultaneously.When treating that the thermal module displays temperature arrives 90 ℃ of reaction temperatures, can collect the cationic wax emulsion finished product from outlet.
Cationic emulsified wax performance indications: white emulsion, solid content 33.7%, PH:5.1.Product stability, 45 ℃, three months outward appearance no changes.
Comparative example 1
With 18g paraffin, the 4g beeswax, 4g palm wax, 1g Span 20 puts into beaker with the 1g hexadecanol, is heated to 80 ℃ of fusings, stirs.5g kation alkyl polysaccharide glycosides is dissolved in 65g water, is heated to 80 ℃.Under the vigorous stirring, oil phase is added dropwise to aqueous phase, adds in the 30min, be warming up to 80 ℃ and under this temperature, be incubated 1h simultaneously.Cooling stops stirring and promptly obtains cationic wax emulsion.
Cationic emulsified wax performance indications: white emulsion, solid content 33.7%, PH:4.65.Product stability, 45 ℃, layering after the week.
Comparative example 2
With 14g paraffin, the 6.5g beeswax, 6.5g palm wax, 1.5g Span 60 puts into beaker with 2g 18 alcohol, is heated to 80 ℃ of fusings, stirs.8g hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride is dissolved in 70g water, is heated to 80 ℃.Under the vigorous stirring, oil phase is added dropwise to aqueous phase, adds in the 30min, be warming up to 90 ℃ and under this temperature, be incubated 1h simultaneously.Cooling stops stirring and promptly obtains cationic wax emulsion.
Cationic emulsified wax performance indications: white emulsion, solid content 35.6%, PH:5.0.Product stability, 45 ℃, layering after the week.
Comparative example 3
With 8g paraffin, the 8g beeswax, 8g palm wax, 2g Span 20 puts into beaker with 3.5g 18 alcohol, is heated to 80 ℃ of fusings, stirs.7.5g lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride is dissolved in 70g water, is heated to 80 ℃.Under the vigorous stirring, oil phase is added dropwise to aqueous phase, adds in the 30min, be warming up to 100 ℃ and under this temperature, be incubated 1h simultaneously.Cooling stops stirring and promptly obtains cationic wax emulsion.
Cationic emulsified wax performance indications: white emulsion, solid content 34.6%, PH:4.7.Product stability, 45 ℃, layering after the week.
Comparative example 4
With 10g paraffin, the 6g beeswax, 6g palm wax, 2.5g Span 60 puts into beaker with the 2g hexadecanol, is heated to 80 ℃ of fusings, stirs.10g lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride is dissolved in 65g water, is heated to 80 ℃.Under the vigorous stirring, oil phase is added dropwise to aqueous phase, adds in the 30min, be warming up to 100 ℃ and under this temperature, be incubated 1h simultaneously.Cooling stops stirring and promptly obtains cationic wax emulsion.
Cationic emulsified wax performance indications: white emulsion, solid content 36.0%, PH:5.Product stability, 45 ℃, three months outward appearance no changes.
(III) performance test
(1) stability test
To be placed on according to the product of the foregoing description and comparative example preparation under 45 ℃ the environment, observe its cosmetic variation.
(2) paintability test
Dispose mixture by following proportioning earlier, roller coat 4g on every foot skin, drying,
50 parts of above-mentioned emulsion;
400 parts of polyaminoester emulsions.
Test softness, permeability and the dried wet rubbing of leather then.
The softness of leather adopts ST300 softness appearance to measure.The numerical value that it is surveyed is between 0-9, and under the same apertures, numerical value is big more, and the skin that representative is surveyed is soft more.
The permeability of leather is judged marking (1-5 branch) through range estimation, and 5=is very good; 4=is good; 3=is general; 2=is bad; 1=is poor.
The xerotripsis performance of leather and wet rubbing performance adopt GB/T4689.20 (or ISO11644) to measure: wear-resisting wiping number of times high-performance more is good more.
Coating leather performance to the product of the foregoing description and comparative example is tested.Test result is shown in Table 1.
Table 1
Can find out that by data in the table emulsion of the embodiment 1 to 5 of method of the present invention preparation has obtained excellent stability under the less situation of emulsifying agent and auxiliary dosage.In addition, adopt the coated leather of emulsion of the present invention, soft good, wet-rub resistance is good, appearance looks elegant, and permeability is good.
And the comparative example 1 to 3 of employing conventional method can't be prepared the stable emulsion product with less emulsifying agent.Though and comparative example 4 can be prepared emulsion, need a large amount of emulsifying agents, can cause in the preparation that a large amount of bubbles is unfavorable for production and processing, also increased production cost simultaneously.In addition, the coated leather of comparative example 4 emulsions, wet-rub resistance is relatively poor, and flexibility is relatively poor, and permeability is bad.
Certainly, the present invention also can have other specific embodiment, more than is merely preferred implementation of the present invention, is not to be used for limiting protection scope of the present invention; Under the situation that does not deviate from spirit of the present invention, those of ordinary skills are every to make various corresponding variations and modification according to content of the present invention, all belongs to the protection domain of claim of the present invention.
Claims (34)
1. a method for preparing emulsion comprises: water composition and hydrophobicity composition are handled in the microreactor system, obtained emulsion.
2. method according to claim 1, wherein, said emulsion comprises: (A) hydrophobicity composition; (B) water; And optional (C) emulsifying agent.
3. method according to claim 2, wherein, said water composition is the aqueous solution that contains emulsifying agent.
4. method according to claim 1, wherein, said hydrophobicity composition is selected from wax, oil, fat, higher alcohols and composition thereof.
5. method according to claim 1, wherein, said hydrophobicity composition is selected from wax, higher alcohols and composition thereof.
6. method according to claim 1, wherein, said hydrophobicity composition comprises wax and higher alcohols.
7. according to each described method of claim 4 to 6, wherein, said wax is selected from biological wax, mineral wax, synthetic wax and composition thereof.
8. according to each described method of claim 4 to 6; Wherein, said wax is selected from paraffin, beeswax, palm wax, spermaceti, ant wax, lanocerin, haze tallow, flax wax, Chinese insect wax, candelila wax, Ka Naba wax, Japan tallow, ore deposit ceresine, ceresine, montanin wax, brown alabaster wax, pertroleum wax, microwax, Fischer-Tropsch wax, Tissuemat E, polypropylene wax, the existing property wax of chemistry, chlorinated paraffin wax, emulsifying wax and composition thereof.
9. according to each described method of claim 4 to 6, wherein, said higher alcohols are C
6～C
24Alkylol.
10. according to each described method of claim 4 to 6; Wherein, said higher alcohols are selected from: hexanol such as n-hexyl alcohol, enanthol such as n-heptanol, octanol such as n-octyl alcohol, nonyl alcohol such as n-nonyl alcohol, decyl alcohol such as Decanol, undecylenic alcohol such as positive undecylenic alcohol, 12 carbon alcohol as positive 12 carbon alcohol, 13 carbon alcohol as positive 13 carbon alcohol, ten four carbon alcohols such as positive ten four carbon alcohols, pentadecanol such as positive pentadecanol, 16 carbon alcohol as positive 16 carbon alcohol, 17 carbon alcohol as positive 17 carbon alcohol, octadecanol such as positive octadecanol, 19 carbon alcohol as positive 19 carbon alcohol, eicosanol such as positive eicosanol, two undecylenic alcohols such as positive two undecylenic alcohols, 22 carbon alcohol as positive 22 carbon alcohol, 23 carbon alcohol as positive 23 carbon alcohol, tetracosa carbon is pure as positive tetracosa carbon alcohol and composition thereof.
11. method according to claim 1, wherein, said hydrophobicity composition comprises grease.
12. according to each described method of claim 2 to 6, wherein, said emulsifying agent is selected from cationic surfactant, anion surfactant, amphoteric surfactant, non-ionic surface active agent and composition thereof.
13. according to each described method of claim 2 to 6, wherein, said emulsifying agent is selected from cationic surfactant, non-ionic surface active agent and composition thereof.
14. method according to claim 12, wherein, said emulsifier package cation surfactant and non-ionic surface active agent perhaps are made up of cationic surfactant and non-ionic surface active agent.
15. method according to claim 12, wherein, said cationic surfactant is selected from one or more in amine salt cationic surfactant, the quaternary cationics.
16. method according to claim 12; Wherein, said cationic surfactant is selected from: kation alkyl polysaccharide glycosides, hexadecanol polyoxyethylene ether dimethyl-octa alkyl ammomium chloride, lauryl alcohol polyoxyethylene ether trimethyl ammonium chloride, imidazoline quaternary ammonium salt, hexadecanol polyoxyethylene ether trimethyl ammonium chloride, polyoxyethylene octadecanol base trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride and composition thereof.
17. method according to claim 1, wherein, said non-surface-active agent is selected from one or more in polyoxyethylene alkane ether, polyoxyethylene fatty acid glyceride, glycol fatty acid ester and the polyoxyethylene fatty acid amine.
18. method according to claim 1; Wherein, Said non-ionic surface active agent is selected from: sorbitan mono-laurate, polyoxyethylene 20 sorbitan monolaurate AEO, polyoxyethylene alkane ether, polyoxyethylene fatty acid glyceride, glycol fatty acid ester, polyoxyethylene fatty acid amine, fatty glyceride and composition thereof.
19. according to each described method of claim 2 to 6, wherein, based on the emulsion gross weight, said emulsifying agent consumption is≤11%.
20. method according to claim 19, wherein, based on the emulsion gross weight, said emulsifying agent consumption is 5%～10%.
21. according to each described method of claim 1 to 6, wherein, based on the emulsion gross weight, solid content is 25%～50%.
22. according to each described method of claim 1 to 6, wherein, based on the emulsion gross weight, said cationic surfactant concentration is 1%～10%.
23. according to each described method of claim 1 to 6, wherein, based on the emulsion gross weight, said non-ionic surfactant concentration is 0.5%～5%.
24. according to each described method of claim 1 to 6, wherein, based on the emulsion gross weight, said higher alcohols content is 0.5%～5%.
25. according to each described method of claim 1 to 6, wherein, based on the emulsion gross weight, solid content is 25%～50%.
26. according to each described method of claim 1 to 6, wherein, based on the emulsion gross weight, solid content is 30%～35%.
27., comprising according to each described method of claim 1 to 6:
(a) with said water composition and the preheating of said hydrophobicity composition;
(b) said water composition and said hydrophobicity composition are handled in the microreactor system, obtained emulsion.
28. method according to claim 27, wherein, in step (a), preheat temperature is to be enough to temperature that all the components is in a liquid state.
29. method according to claim 28, wherein, said preheat temperature is 60～100 ℃.
30. method according to claim 1, wherein, said microreactor system comprises reactor, and wherein temperature of reactor is more than or equal to preheat temperature.
31. the emulsion that obtains according to each described method of claim 1 to 30.
32. a leather nursing emulsion comprises:
(i) emulsion according to claim 31;
(ii) other leather finish auxiliary agents.
33. leather nursing emulsion according to claim 32, wherein, said other leather finish auxiliary agents are selected from one or more in polyaminoester emulsion, polyacrylic acid emulsion, the nitrocotton emulsion.
34. applying or nursing the purposes in the leather and fur products according to claim 32 or 33 described leather nursing emulsions.
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| PCT/CN2013/070544 WO2013107348A1 (en) | 2012-01-18 | 2013-01-16 | Emulsion preparation method and leather care emulsion, and use thereof |
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|---|---|
| WO2013107348A1 (en) | 2013-07-25 |
| CN102553504B (en) | 2014-12-17 |
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Effective date of registration: 20210816 Address after: 213127 No. 318, Huanghai Road, Xinbei District, Changzhou City, Jiangsu Province Patentee after: Shengrui (Changzhou) special materials Co.,Ltd. Address before: 213127 No. 8, Huanghai Road, Xinbei District, Changzhou City, Jiangsu Province Patentee before: LANXESS (CHANGZHOU) Co.,Ltd. |
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Address after: 213127 No. 318, Huanghai Road, Xinbei District, Changzhou City, Jiangsu Province Patentee after: TFL (Changzhou) Co.,Ltd. Address before: 213127 No. 318, Huanghai Road, Xinbei District, Changzhou City, Jiangsu Province Patentee before: Shengrui (Changzhou) special materials Co.,Ltd. |