CN101446038A - Brightening agent for fabrics and production method thereof - Google Patents
Brightening agent for fabrics and production method thereof Download PDFInfo
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Abstract
The invention discloses a brightening agent for fabrics, which comprises the use of amino-silicone oil and is characterized in that N-(beta-aminoethyl)-gamma-aminopropyl methyl dimethoxy silane functional groups are introduced to the structure of the amino-silicone oil. The production method of the brightening agent for the fabrics adopts the polymerization of octamethylcyclotetrasiloxane or the mixture of methyl cyclic siloxane, or linear hydroxy-terminated polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxy silane for preparing the amino-silicone oil under the action of a catalyst, then the amino-silicone oil is emulsified to emulsion of a water system under the action of a surfactant, and cationic polyurethane emulsion or cationic acrylic resin emulsion with a certain proportion is further added. The technical effects are as follows: the product stability is excellent; the brightening agent has significant brightening role after being used on natural fabrics and synthetic fabrics, the color light level is improved by 4 to 5 levels, and the brightening agent has no emission pollution, thereby being in line with the requirements of environmental protection; and the brightening agent can also improve the smooth and soft hand feel of the fabrics.
Description
Technical field
The present invention relates to production method of a kind of textile auxiliary, particularly a kind of brightening agent for fabrics and products thereof.
Background technology
Along with the continuous appearance of weaving new product, textile auxiliary market also will develop rapidly.Along with entry into the World Trade Organization back textile exports quota is phased out, the outlet of China's textiles also will obtain certain growth, and therefore the demand to textile auxiliary also can correspondingly increase.Along with people more and more pay close attention to green textiles and environmental and ecological protection, the environment-friendly type textile auxiliary has become the main direction of current textile auxiliary development.International Textile ecological study and check association explicitly call for, and textile auxiliary also need satisfy the requirement of environment-friendly quality except will possessing necessary use technology applicability, application performance and firm performance.
At present, because a large amount of uses of homemade dyestuff, and a large amount of appearance of new structure lining are in actual production process, fabric color after the dyeing is bright-coloured inadequately, the burnt hair obfuscation causes the class of lining product to reduce, and competitiveness descends, dye level is high more in fact, light fastness is also good more, and when dying light color, light fastness is often defective.Though and existing silicone based or non-silicon class deep-dyeing agent, brightening agent can make moderate progress to shade fabric on the market, but it is poor to increase dark brightening effect, increase the general ruddiness of dark light, fabrics smooth, soft feel are poor, the product stability shortcoming, still can not reach promising result, and fabric through repeatedly the washing after color and luster obviously descend, lose usefulness.Along with the increase day by day of textile exports amount and the quick growth of domestic consumption market, textile industry is also increasing to the demand of this product, also product has been proposed to meet environmental protection requirement simultaneously.Therefore, the domestic research and development that must strengthen to fabric brightening agent auxiliary agent, develop high-effect, environmental protection, durability is strong, and the corresponding product that fabric feeling is increased.
Summary of the invention
The objective of the invention is to provide a kind of pliability, smoothness good, increase that to increase gorgeous degree height, washability, compatibility deeply strong for the deficiency that solves above-mentioned technology, and the production method of the brightening agent for fabrics of the brightening agent of high-efficiency environment friendly and products thereof.
In order to achieve the above object, brightening agent for fabrics provided by the invention, it comprises the employing amido silicon oil, it is characterized in that introducing on the amido silicon oil structure N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group.
In order to achieve the above object, a kind of above-mentioned fabrics provided by the invention production method of brightening agent, be that employing octamethylcy-clotetrasiloxane or methyl ring siloxane mixture or linear hydroxyl endblocked polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxysilane aggregate into a kind of amido silicon oil under catalyst action, under the effect of surfactant, be emulsified into the emulsion of aqueous systems then, add a certain proportion of polyurethane/cationic fat resin emulsion or acrylic cationic resin emulsion again, promptly obtain brightening agent for fabrics of the present invention.At this, described catalyst can be potassium hydroxide or tetramethyl oxyammonia.
The production method of described brightening agent for fabrics, its technical process is as follows:
The first step: in octamethylcy-clotetrasiloxane or methyl ring siloxane mixture or linear hydroxyl endblocked polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxysilane adding reactor, adding catalyst stirring intensification reacts, adding neutralizer after reaction is finished neutralizes, drive vavuum pump after the neutralization unreacted methyl cyclosiloxane is deviate from, obtain a kind of amido silicon oil; Wherein:
Polymeric reaction temperature: 140 ℃～160 ℃ polymerization reaction times: 4 hours～6 hours
Neutralization reaction temperature: 140 ℃～160 ℃ neutralization reaction times: 2 hours～4 hours
Take off low reaction temperatures: 140 ℃～160 ℃ are taken off the low reaction time: 2 hours～4 hours
Mixing speed: 200rpm～600rpm takes off rough vacuum :-0.1MPa
Octamethylcy-clotetrasiloxane and aminoethyl aminopropyl methyl dimethoxysilane weight ratio=1000:2～4
Octamethylcy-clotetrasiloxane and catalyst weight ratio=1000:0.05～0.2
Octamethylcy-clotetrasiloxane and neutralizer weight ratio=1000:0.25～1.0
The viscosity of amido silicon oil: 30000CS～150000CS
The ammonia value (percentage by weight) of amido silicon oil: 0.4%～0.6%
Second step: amido silicon oil, pure water, collateralization C13 polyoxyethylene ether 5EO emulsifying agent, collateralization C13 polyoxyethylene ether 7EO emulsifying agent that first step reaction is generated add in the emulsion reactor, carry out emulsification with the high speed shear mulser, after emulsification is finished, add glacial acetic acid and be neutralized to pH value 6～7.
Wherein: emulsifying temperature: ≦ 50 ℃ emulsification times: 1～2 hour pH value: 6～7
Amido silicon oil and pure water weight ratio=100:330～360
Amido silicon oil and collateralization C13 polyoxyethylene ether 5EO emulsifying agent weight ratio=100:1.6～3.2
Amido silicon oil and collateralization C13 polyoxyethylene ether 7EO emulsifying agent weight ratio=100:1.6～3.2
Amido silicon oil and glacial acetic acid weight ratio=100:0.1～0.3
The 3rd step: the emulsion after the second step emulsification is moved in the homogenizer, with emulsion homogenizer emulsification 3 times.Add crosslinking agent again, obtain product efficient and environment-friendly type brightening agent;
Wherein: second emulsifying temperature: ≦ 60 ℃ of second emulsifying pressure: 30MPa～40MPa
The second emulsifying time: 1 hour～2 hours
Emulsion and crosslinking agent weight ratio=1000:40～60.
Described neutralizer can be certain herbaceous plants with big flowers acid or carbon dioxide, and described crosslinking agent can be polyurethane/cationic fat resin emulsion or acrylic cationic resin emulsion.
Brightening agent for fabrics provided by the invention, after using on natural fabric and the chemical ﹠ blended fabric, have to increase significantly and increase gorgeous effect deeply, the coloured light grade improves the 4--5 level, on average can save dye dosage 24.3%, even before not using this product originally, add amount of dye than positive usual amounts into 24.3%, also can't reach the effect of using behind this product.
Can improve simultaneously level and smooth, the soft feel of fabric, owing to adopted the trifunctional structure of many groups such as polyurethane/cationic fat resin emulsion or acrylic cationic resin emulsion, washability on fabric is splendid, and after 50 washings, fabric still can keep not washing preceding 96% color and luster.
Particularly, its technique effect is:
1, adopt the method for structurally introducing small amount of N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group to produce brightening agent, the synthesis technique uniqueness, product stability is splendid.
2, after using on natural fabric and the chemical ﹠ blended fabric, have to increase significantly and increase gorgeous effect deeply, the coloured light grade improves the 4--5 level, on average can save dye dosage 24.3%, even before not using this product originally, add amount of dye than positive usual amounts, also can't reach the effect of using behind this product into 24.3%.
3, the group of unfavorable environmental protection such as this product AZO, phenol, fabric are to working solution absorptivity height, and no emission performance pollutes, and biological degradability own is good, can also directly reduce dye for fabrics consumption, very compliance with environmental protection requirements.
4, improve level and smooth, the soft feel of fabric, owing to adopted the trifunctional structure of many groups, the washability on fabric is splendid, and after 50 washings, fabric still can keep not washing preceding 96% color and luster.
5, finished the pilot scale work of project, determined best postfinishing process, simultaneously according to the difference of facing fabric (as cotton, polyester-cotton blend, wool, fiber crops, silk, wash, blending etc.), suitable product processes parameter and prescription have been found out, for large-scale industrial production provides reliable assurance.
Description of drawings
Fig. 1 is an embodiment of the invention process flow diagram.
The specific embodiment
The invention will be further described in conjunction with the accompanying drawings below by embodiment.
Embodiment:
Brightening agent for fabrics provided by the invention, it comprises the employing amido silicon oil, it is characterized in that introducing on the amido silicon oil structure N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group.
As shown in Figure 1, the production method of brightening agent for fabrics provided by the invention is to adopt octamethylcy-clotetrasiloxane or linear hydroxyl endblocked polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxysilane to aggregate into a kind of amido silicon oil under catalyst action, under the effect of surfactant, be emulsified into the emulsion of aqueous systems then, add a certain proportion of polyurethane/cationic fat resin emulsion or acrylic cationic resin emulsion again, be brightening agent for fabrics of the present invention.At this, described catalyst is selected potassium hydroxide for use.
Its technical process is as follows:
The first step: in octamethylcy-clotetrasiloxane or methyl ring siloxane mixture or linear hydroxyl endblocked polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxysilane adding emulsion reactor, add catalyst potassium hydroxide or tetramethyl oxyammonia, stirring heats up reacts, adding glacial acetic acid after reaction is finished neutralizes, drive vavuum pump after the neutralization unreacted methyl cyclosiloxane is deviate from, obtain a kind of amido silicon oil; Wherein:
Polymeric reaction temperature: 140 ℃ of polymerization reaction times: 4 hours
Neutralization reaction temperature: 140 ℃ of neutralization reaction times: 2 hours
Take off low reaction temperatures: 140 ℃ are taken off the low reaction time: 2 hours
Mixing speed: 200rpm takes off rough vacuum :-0.1MPa
Octamethylcy-clotetrasiloxane and aminoethyl aminopropyl methyl dimethoxysilane weight ratio=1000:2
Octamethylcy-clotetrasiloxane and catalyst weight ratio=1000:0.05
Octamethylcy-clotetrasiloxane and neutralizer weight ratio=1000:0.25
The viscosity of amido silicon oil: 30000CS
The ammonia value (percentage by weight) of amido silicon oil: 0.4%
Second step: amido silicon oil, pure water, collateralization C13 polyoxyethylene ether 5EO emulsifying agent, collateralization C13 polyoxyethylene ether 7EO emulsifying agent that first step reaction is generated add in the emulsion reactor, carry out emulsification with the high speed shear mulser, after emulsification is finished, add glacial acetic acid and be neutralized to pH value 6.
Wherein: emulsifying temperature: ≦ 50 ℃ emulsification times: 1 hour pH value: 6
Amido silicon oil and pure water weight ratio=100:330
Amido silicon oil and collateralization C13 polyoxyethylene ether 5EO emulsifying agent weight ratio=100:1.6
Amido silicon oil and collateralization C13 polyoxyethylene ether 7EO emulsifying agent weight ratio=100:1.6
Amido silicon oil and glacial acetic acid weight ratio=100:0.1
The 3rd step: the emulsion after the second step emulsification is moved in the homogenizer, with emulsion homogenizer emulsification 3 times.Add crosslinking agent polyurethane/cationic fat resin emulsion again, obtain product efficient and environment-friendly type brightening agent.
Wherein: second emulsifying temperature: ≦ 60 ℃ of second emulsifying pressure: 30～40MPa
The second emulsifying time: 1～2 hour
Emulsion and crosslinking agent weight ratio=1000:40.
The brightening agent for fabrics that present embodiment obtains, its product technology parameter:
Outward appearance: milky white liquid
PH value: 5-7
Solid content (105 ℃ * 2hr) 〉=27%
Dispersed: in soluble in water
Embodiment 2:
The production method of the brightening agent that present embodiment is described, be to adopt methyl ring siloxane mixture and aminoethyl aminopropyl methyl dimethoxysilane under catalyst action, to aggregate into a kind of amido silicon oil, under the effect of surfactant, be emulsified into the emulsion of aqueous systems then, add a certain proportion of polyurethane/cationic fat resin emulsion or acrylic cationic resin emulsion again, be brightening agent for fabrics of the present invention.At this, described catalyst is selected the tetramethyl oxyammonia for use.
Its technical process is as follows:
The first step: methyl ring siloxane mixture and aminoethyl aminopropyl methyl dimethoxysilane are added in the emulsion reactor, add catalyst tetramethyl oxyammonia, stirring heats up reacts, adding the neutralizer carbon dioxide after reaction is finished neutralizes, drive vavuum pump after the neutralization unreacted methyl cyclosiloxane is deviate from, obtain a kind of amido silicon oil; Wherein:
Polymeric reaction temperature: 160 ℃ of polymerization reaction times: 6 hours
Neutralization reaction temperature: 160 ℃ of neutralization reaction times: 4 hours
Take off low reaction temperatures: 160 ℃ are taken off the low reaction time: 4 hours
Mixing speed: 600rpm takes off rough vacuum :-0.1MPa
Octamethylcy-clotetrasiloxane and aminoethyl aminopropyl methyl dimethoxysilane weight ratio=1000:4
Octamethylcy-clotetrasiloxane and catalyst weight ratio=1000:0.2
Octamethylcy-clotetrasiloxane and neutralizer weight ratio=1000:1.0
The viscosity of amido silicon oil: 150000CS
The ammonia value (percentage by weight) of amido silicon oil: 0.6%
Second step: amido silicon oil, pure water, collateralization C13 polyoxyethylene ether 5EO emulsifying agent, collateralization C13 polyoxyethylene ether 7EO emulsifying agent that first step reaction is generated add in the emulsion reactor, carry out emulsification with the high speed shear mulser, after emulsification is finished, add carbon dioxide and be neutralized to pH value 6～7.
Wherein: emulsifying temperature: ≦ 50 ℃ emulsification times: 2 hours pH values: 7
Amido silicon oil and pure water weight ratio=100:360
Amido silicon oil and collateralization C13 polyoxyethylene ether 5EO emulsifying agent weight ratio=100:3.2
Amido silicon oil and collateralization C13 polyoxyethylene ether 7EO emulsifying agent weight ratio=100:3.2
Amido silicon oil and glacial acetic acid weight ratio=100:0.3
The 3rd step: the emulsion after the second step emulsification is moved in the homogenizer, with emulsion homogenizer emulsification 3 times.Add crosslinking agent acrylic cationic resin emulsion again, obtain product efficient and environment-friendly type brightening agent.
Wherein: second emulsifying temperature: ≦ 60 ℃ of second emulsifying pressure: 40MPa
The second emulsifying time: 2 hours
Emulsion and crosslinking agent weight ratio=1000:60.
In order further to be familiar with and to understand flesh and blood of the present invention, below technology contents of the present invention is made further analysis introduction:
(1), the silane functionality group determines
According to data check and market survey, we adopt the method for structurally introducing small amount of N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group, compare with amido silicon oil constructed products general on the market, the product of methyl-silicone oil deep-dyeing agent.Find to adopt general amido silicon oil constructed products, pliability is fine, and the fabric coloured light that is organized is changed, and presents ruddiness, and glossiness weakens; Methyl-silicone oil deep-dyeing agent product then has the emulsion instability, and it is not remarkable to increase dark effect, and the shortcoming that feel is not good is handled unless carry out feel more separately, but can be made production process complicated, and production efficiency reduces, and production cost rises; And the product that the method that adopts introducing small amount of N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group is produced, can well solve the stability of emulsion, have excellent dark, the brightening effect of increasing simultaneously, increase the gloss of fabric, eliminated the phenomenon of the general ruddiness of common deep-dyeing agent, obviously improve the class and the quality of fabric, make fabric have well level and smooth, soft feel simultaneously, reached multi-functional requirement.
Therefore, we determine that it is agent structure that small amount of N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group is structurally introduced in employing.
(2), functional polyorganosiloxane group determination of ratio
Determined the composition of functional polyorganosiloxane group, we then carry out the experiment of functional polyorganosiloxane group ratio.We take into account the process complexity of product by a large amount of synthetic and application experiments, operability, and comprehensive feel increases dark degree, and problems such as coloured light color and luster intensity of variation and manufacturing cost have been determined best prescription and synthesis technique.Find to adopt the ratio (weight ratio) of octamethylcy-clotetrasiloxane and aminoethyl aminopropyl methyl dimethoxysilane weight ratio=1000:2～4, its combination property is best.The ratio of aminoethyl aminopropyl methyl dimethoxysilane weight ratio improves, and make fabric increase dark degree and improve, but cost raises; The ratio of aminoethyl aminopropyl methyl dimethoxysilane weight ratio reduces, and cause fabric to increase dark degree and reduce, and the poor stability of product, oil spill easily.Therefore, we determine to adopt the ratio of octamethylcy-clotetrasiloxane and aminoethyl aminopropyl methyl dimethoxysilane weight ratio=1000:2～4.
(3), the emulsifying agent composition determines
Emulsifying agent is formed:
According to data check and market survey, we adopt collateralization polyoxyethylene ether special surfactant, carry out emulsifiability relatively with surfactants such as C12-C15 fatty alcohol-polyoxyethylene ether general on the market, alkylphenol polyoxyethylene.Find that collateralization polyoxyethylene ether special surfactant has the characteristic that efficient oversubscription is loose, the consumption of available silicone oil below 10% reaches high product stability, and the electrolyte-resistant performance is strong, so just can reduce the side effect of surfactant, improve adsorptivity and the film forming of Main Ingredients and Appearance organosilicon functional group on fabric comprehensively, the effect that has greatly improved the product effective ingredient strengthens, effective ingredient is played a role, help the reduction of use cost, avoided the pollution of surfactant in the working solution and organosilicon composition environment.And common softener employing is the C12-C15 fat alcohol polyethylene ether of using always, surfactants such as alkylphenol polyoxyethylene, emulsifying effectiveness is poor, consumption big (consumption is 50% usually), hindered adsorptivity and the film forming of organosilicon functional group on fabric, can't give full play to the effect of effective ingredient in the product, and cause production cost to raise, the product utilization rate descends.Therefore, we determine to adopt collateralization polyoxyethylene ether special surfactant as selected emulsifying agent.
The influence of emulsifier proportion:
Determined the composition of emulsifying agent, we then carry out the experiment of emulsifier proportion.Find to adopt emulsifying agent: the ratio of organosilicon main component=3～6:100 (weight ratio), the product stability height, the electrolyte-resistant performance is strong, pliability, flatness, fine and smooth sense, glossiness and increase dark effect and be significantly improved.And the ratio of emulsifying agent reduces, and product stability variation, electrolyte-resistant performance be variation also; The ratio of emulsifying agent improves, and product stability and electrolyte-resistant performance do not have obvious raising, but the coloured light of fabric is had adverse effect, are easy to generate the aberration of inclined to one side redness.Therefore, we determine to adopt amido silicon oil and collateralization C13 polyoxyethylene ether 5EO emulsifying agent weight ratio=100:1.6～3.2, amido silicon oil and collateralization C13 polyoxyethylene ether 7EO emulsifying agent weight ratio=100:1.6～3.2.
(4), production technology determines
In first step polymerisation:
Polymerisation has two kinds of reaction process, as adopt potassium hydroxide or tetramethyl oxyammonia to make catalyst, when adopting potassium hydroxide to make catalyst, reaction temperature is at 140～160 ℃, reaction time was at 4～6 hours, in and the time can adopt the neutralization of certain herbaceous plants with big flowers acid or carbon dioxide neutralizer, such process route cost is low, the product odorlessness.
Another kind is to adopt the tetramethyl oxyammonia to make catalyst, and reaction temperature is at 80 ℃～95 ℃, and the reaction time was at 4 hours～6 hours, in and the time neutralize without neutralizer, can be warmed up to 140 ℃～160 ℃ decomposition catalysts, such process route is convenient, but some smell of product.
In the second step emulsion reaction:
The emulsifying temperature of reactant remains on normal temperature the best, but material is under the effect of high-speed emulsifying machine, because the effect of mechanical shear stress, cause material to produce temperature rise, but learn that by experiment emulsifying temperature surpasses when being 55 ℃, the unstability of pre-emulsified body obviously improves.And to control emulsification under the low temperature, then cost has and significantly improves, and process complexity improves.Temperature is controlled at below 50 ℃, and is little to the stability influence of pre-emulsified body.Therefore, we consider temperature Change and material from the temperature rise situation, the decision temperature of emulsification is controlled at below 50 ℃.
During once pre-emulsification treatment material, adding water speed will control well, at the uniform velocity carries out, and adds the water time to be controlled at about 45 minutes, it is too fast to add water speed, can cause emulsified body phase inversion inequality, and particle is too big, it is too slow to add water speed, can cause the phase inversion process temperature too high, is unfavorable for the formation of stable emulsified body; Total emulsification treatment time should be controlled at 1～2 hour, and the long time can cause the temperature of emulsified body too high, is unfavorable for the formation of stable emulsified body.
In the 3rd step second emulsifying:
The pre-emulsification of the secondary of reactant is with once pre-emulsified principle is the same, and temperature remains on normal temperature the best, but material is under the effect of homogenizer, cause material to produce temperature rise, but learn that by experiment emulsifying temperature surpasses when being 65 ℃, the unstability of pre-emulsified body obviously improves.Temperature is controlled at below 60 ℃, and is little to the stability influence of pre-emulsified body.Therefore, we consider temperature Change and material from the temperature rise situation, the decision the pre-emulsified temperature of secondary is controlled at below 60 ℃.
During the pre-emulsification of secondary, the operating pressure of homogenizer is controlled at 30MPa～40MPa, and homogeneous gets final product for three times, and too high pressure and increase the homogeneous number of times particle diameter of emulsified body is further diminished has increased the production time on the contrary meaninglessly; Cross low pressure and then can make the particle diameter of emulsified body too big, be unfavorable for the carrying out of polymerisation with minimizing homogeneous number of times.
Claims (5)
1, a kind of brightening agent for fabrics, it comprises the employing amido silicon oil, it is characterized in that introducing on the amido silicon oil structure N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane functional group.
2, a kind of production method according to the described brightening agent for fabrics of claim 1, it is characterized in that adopting octamethylcy-clotetrasiloxane or methyl ring siloxane mixture or linear hydroxyl endblocked polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxysilane under catalyst action, to aggregate into a kind of amido silicon oil, under the effect of surfactant, be emulsified into the emulsion of aqueous systems then, add polyurethane/cationic fat resin emulsion or the acrylic cationic resin emulsion of determining ratio again, obtain brightening agent for fabrics of the present invention.
3, the production method of described brightening agent for fabrics according to claim 2 is characterized in that described catalyst is potassium hydroxide or tetramethyl oxyammonia.
4,, it is characterized in that technical process is as follows according to the production method of claim 2 or 3 described brightening agent for fabrics:
The first step: in octamethylcy-clotetrasiloxane or methyl ring siloxane mixture or linear hydroxyl endblocked polydimethylsiloxane and aminoethyl aminopropyl methyl dimethoxysilane adding reactor, adding catalyst stirring intensification reacts, adding neutralizer after reaction is finished neutralizes, drive vavuum pump after the neutralization unreacted methyl cyclosiloxane is deviate from, obtain a kind of amido silicon oil; Wherein:
Polymeric reaction temperature: 140 ℃～160 ℃ polymerization reaction times: 4 hours～6 hours
Neutralization reaction temperature: 140 ℃～160 ℃ neutralization reaction times: 2 hours～4 hours
Take off low reaction temperatures: 140 ℃～160 ℃ are taken off the low reaction time: 2 hours～4 hours
Mixing speed: 200～600rpm takes off rough vacuum :-0.1MPa
Octamethylcy-clotetrasiloxane and aminoethyl aminopropyl methyl dimethoxysilane weight ratio=1000:2～4
Octamethylcy-clotetrasiloxane and catalyst weight ratio=1000:0.05～0.2
Octamethylcy-clotetrasiloxane and neutralizer weight ratio=1000:0.25～1.0
The viscosity of amido silicon oil: 30000CS～150000CS
The ammonia value (percentage by weight) of amido silicon oil: 0.4%～0.6%
Second step: amido silicon oil, pure water, collateralization C13 polyoxyethylene ether 5EO emulsifying agent, collateralization C13 polyoxyethylene ether 7EO emulsifying agent that first step reaction is generated add in the emulsion reactor, carry out emulsification with the high speed shear mulser, after emulsification is finished, add glacial acetic acid and be neutralized to pH value 6～7;
Wherein: emulsifying temperature: ≦ 50 ℃ emulsification times: 1 hour～2 hours pH values: 6～7
Amido silicon oil and pure water weight ratio=100:330～360
Amido silicon oil and collateralization C13 polyoxyethylene ether 5EO emulsifying agent weight ratio=100:1.6～3.2
Amido silicon oil and collateralization C13 polyoxyethylene ether 7EO emulsifying agent weight ratio=100:1.6～3.2
Amido silicon oil and glacial acetic acid weight ratio=100:0.1～0.3
The 3rd step: the emulsion after the second step emulsification is moved in the homogenizer, emulsion with homogenizer emulsification 3 times, is added crosslinking agent again, obtain the brightening agent for fabrics of product efficient and environment-friendly type;
Wherein: second emulsifying temperature: ≦ 60 ℃ of second emulsifying pressure: 30MPa～40MPa
The second emulsifying time: 1 hour～2 hours
Emulsion and crosslinking agent weight ratio=1000:40～60.
5, the production method of described brightening agent for fabrics according to claim 4 is characterized in that described neutralizer is certain herbaceous plants with big flowers acid or carbon dioxide; Described crosslinking agent adopts polyurethane/cationic fat resin emulsion or acrylic cationic resin emulsion.
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| CN100543068C (en) * | 2006-06-20 | 2009-09-23 | 浙江大学 | A kind of preparation method of nano grade amino silicon oil emulsion |
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