CN104693343A - Preparation method of emulsification slurry used for weaving - Google Patents
Preparation method of emulsification slurry used for weaving Download PDFInfo
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- CN104693343A CN104693343A CN201310653151.2A CN201310653151A CN104693343A CN 104693343 A CN104693343 A CN 104693343A CN 201310653151 A CN201310653151 A CN 201310653151A CN 104693343 A CN104693343 A CN 104693343A
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Abstract
The invention relates to a preparation method of an emulsion nano composite acrylic acid copolymerization slurry, the slurry is composited by the acrylic acid copolymerization slurry and an inorganic material on a nanoscale size, and solid content is 10-50%. The method comprises the following steps: weighing clay and adding in water, adjusting the pH value, stirring the clay to form a uniform dispersion liquid; weighing an oil solubility monomer to blend an oil solubility mixing monomer solution; weighing a water-soluble monomer and adding in water for dissolving, adjusting the pH value by alkali to obtain a water-soluble mixing monomer solution; then respectively adding the oil solubility mixing monomer solution and the water-soluble mixing monomer solution in the clay dispersion liquid, adding an emulsifier and an initiator, uniformly stirring, heating for initiating a copolymerization reaction, adding residual oil solubility monomer mixing solution and the water-soluble monomer mixing solution drop by drop, insulating until the reaction is complete, heating and continuously reacting until no monomer flows back, cooling and adjusting the pH value, and filtering to obtain the product. The method has the advantages of simple technology and good performance.
Description
Technical field:
The invention belongs to textile raw material preparing technical field, relate to a kind of preparation method of emulsion nano composite acrylic acid copolymerization slurry.
Technical background:
As everyone knows, spinning sizing agent is mainly divided into Starch Size, polyvinyl alcohol (PVA) slurry and polyacrylic size three major types.Polyvinyl alcohol pulp is after first time in 1940 is used for warp sizing, owing to having excellent film-forming properties, adhesivity and the feature good with other slurry intermiscibility, adopted by textile industry soon, after synthon union yarn (washing/cotton) comes out, PVA slurry also can meet its starching requirement.At present in textile warp sizing process, PVA has been widely used in cotton textiles as main slurry, polyester-cotton blend, the starching of washing the yarns such as sticky, polyamide fibre use, and be considered to desirable slurry.But along with the reinforcement of environmental protection consciousness, developed country in recent years, the particularly Western European countries are difficult to biological degradation for PVA slurry, and cause the present situation of severe contamination to environment, have proposed to prohibit the use PVA as spinning sizing agent.China also proposed in 1997 the slurry developing goal using no or little PVA in sizing process.But even to this day, the progress both at home and abroad in substitution for PVA slurry is little, thus uses no or little the developing direction that PVA remains China's spinning sizing agent in recent years.
Acrylic size is commonly called as " tailor " slurry, due to the designability of its stuctures and properties, thus can meet the requirement of different yarns sizing performance, such slurry is easy to flocculation, reclaims and be biodegradable in desized wastewater simultaneously, is therefore also considered to eco-friendly spinning sizing agent.But because the production cost of such slurry is higher, therefore can only be used as auxiliary slurry and be used for all kinds of yarn sizing, Some substitute PVA slurry.
Nano composite material is the type material that development in recent years is got up, and is called as one of " 21 century the most promising material " ". nano composite material refers to that dispersed phase size has at least the one dimension size of a phase to be less than the matrix material of 100nm. Preparing Organic-inorganic Nano Hybrid Material is that inorganic nanostructures unit is scattered in the matrix material formed in polymeric matrix.Inorganic materials has excellent heat resistance and flame retardant resistance, high strength, high rigidity, and polymer materials has good snappiness, by bi-material compound on nanoscale, just can the advantage of conjugated polymer and inorganic nano material, thus improve the mechanical property of polymkeric substance significantly.Inorganic materials and acrylic size are carried out compound on nanoscale and prepares nano composite acrylic acid slurry, also likely improve the sizing performance of existing acrylic size.
Summary of the invention:
The object of the invention is to overcome the shortcoming existed in prior art, seek emulsion nano composite acrylic acid copolymerization slurry that a kind of eco-friendly is provided and preparation method thereof, it and modified starch size with the use of, can substitution for PVA slurry completely in the sizing process of polyester-cotton blend or polyester/rayon yarns line, the existing slashing technique of textile enterprise causes environmental pollution deficiency because using PVA slurry can be overcome.
In order to realize foregoing invention object, emulsion nano composite acrylic acid copolymerization slurry provided by the invention, be composited by acrylic acid copolymerization slurry and inorganic materials on nano-grade size, its solid content is 10-50%; Wherein said inorganic materials is clay, comprises sodium bentonite, sodium-based montmorillonite, kaolin, halloysite, and its clay content accounts for the 1-30% of acrylic acid copolymerization slurry butt weight; The mix monomer that the said acrylic acid copolymerization slurry of the present invention is made up of two or more third vinyl monomer or vinyl monomer is that solvent is reacted by emulsion copolymerization and prepares with water; The third described vinyl monomer or vinyl monomer comprise vinylformic acid, acrylamide, vinyl cyanide, vinyl acetate, methyl acrylate, ethyl propenoate, butyl acrylate, methacrylic acid, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, vinylbenzene.
The emulsion nano composite acrylic acid copolymerization slurry preparation method that the present invention proposes, implements: first take clay and be added to the water, adjust ph is 6-9 in the steps below, stirs and makes clay form uniform dispersion liquid, take oil-soluble monomer configuration oil soluble mixed monomer solution again, and take water-soluble monomer and be added to the water dissolving, be 3-7 by alkali adjust ph, obtain water-soluble mixed monomer solution, then in clay dispersion, add the water-soluble mixed monomer solution of the oil soluble mixed monomer solution of 10-50% and the 10-50% of equivalent respectively, add the initiator of the emulsifying agent of the 0.5-5% of water-soluble and oil-soluble monomer total amount and the 0.1-2.5% of water-soluble and oil-soluble monomer total amount again, stir, be warming up to 30-85 DEG C and cause copolyreaction, when in reaction solution, mix monomer primitive reaction is complete, start to drip surplus oil dissolubility mix monomer and water-soluble monomer mixing solutions respectively simultaneously, dripped within 3 hours, at 30-85 DEG C, insulation reaction is complete to mix monomer primitive reaction, be warming up to 90-95 DEG C, continue reaction to monomer-free to reflux, be cooled to less than 50 DEG C, adjust ph is 5-7, filter, obtain emulsion nano composite acrylic acid copolymerization slurry.
Clay of the present invention is sodium bentonite or sodium-based montmorillonite or kaolin or halloysite, and its content accounts for the 1-30% of acrylic acid or the like mix monomer gross weight; Described initiator is persulphate, comprises ammonium persulphate or Potassium Persulphate, or the redox initiator that persulphate forms with sodium bisulfite or S-WAT; Described oil soluble mixed monomer solution comprises one or more monomers composition in vinyl acetate, methyl acrylate, ethyl propenoate, butyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, vinylbenzene; Described water-soluble mix monomer comprises one or more monomers composition in vinylformic acid, acrylamide, vinyl cyanide, methacrylic acid; Described emulsifying agent refers to by one or both in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, polyoxyethylene nonylphenol ether or two or morely to form.
The present invention adopts emulsion polymerization in situ to be that inorganic materials prepares emulsion nano composite acrylic acid copolymerization slurry with clay.In preparation process, in order to make, preparation is simple, carries out in-situ emulsion polymerization reaction under not adopting nitrogen protection.But preparation technology of the present invention can successfully implement completely under nitrogen protection.Emulsion nano composite acrylic acid copolymerization slurry prepared by the present invention can improve the sizing performance of existing acrylic size, and be easy to biological degradation, for Eco-friendly spinning sizing agent, this slurry and modified starch size are with the use of to polyester-cotton blend yarn and the starching of polyester/rayon yarns line, there is excellent sizing performance, and can size mixing technology be simplified, significantly reduce sizing costs.Successful great advantage developed by this slurry is to overcome a large amount of environmental pollution using PVA slurry to cause in current textile enterprise's sizing production technique both at home and abroad.
Embodiment:
Embodiments of the present invention are further illustrated below by embodiment.
Embodiment 1: the preparation of emulsion nano composite acrylic acid copolymerization slurry A
Taking 5g sodium bentonite adds in 85ml water, is 8 by alkali lye adjust ph, and stirring to pulp prepares sodium bentonite dispersion liquid in 1 hour.Taking vinylformic acid 2.5g adds in 22ml water, neutralizes to obtain water-soluble mixed monomer solution with 0.8g sodium hydroxide, take butyl acrylate 30g, vinyl-acetic ester 12.5g, be mixed to get oil-soluble monomer mixing solutions, 1/5th of water-soluble mixed monomer solution total amount and 1/5th of oil soluble mixed monomer solution total amount are added respectively in the sodium bentonite dispersion liquid that stirred, add 1g polyoxyethylene nonylphenol ether and 0.2g sodium laurylsulfonate, stir, add 0.5g ammonium persulphate again, continue stir and be slowly warming up to reflux temperature initiation reaction, when keeping reflux temperature continuation reaction to reaction solution backflow substantially to disappear, start evenly to drip surplus oil dissolubility mix monomer and water-soluble monomer mixing solutions, reflux temperature is kept all to add to monomer, after monomer all adds, continue to keep reflux temperature to reacting liquid temperature to rise to 90 DEG C, and after backflow disappearance, stopped reaction, cooling, adjust ph is 6-7, filter with gauze, obtain the water-soluble nano composite acrylic acid copolymerization slurry A that solid content is about 30%.
Embodiment 2: the preparation of emulsion nano composite acrylic acid copolymerization slurry B
Implementation process, with embodiment 1, just changes 5g sodium bentonite into 8g sodium-based montmorillonite, changes 85ml water into 82ml, can obtain the emulsion nano composite acrylic acid copolymerization slurry B that solid content is about 30%.
Embodiment 3: the preparation of emulsion nano composite acrylic acid copolymerization slurry C
Implementation process, with embodiment 1, just changes 5g sodium bentonite into 10g halloysite, changes 85ml water into 80ml, can obtain the emulsion nano composite acrylic acid copolymerization slurry C that solid content is about 30%.
Respectively emulsion nano composite acrylic acid copolymerization slurry A, B and C of above-mentioned preparation are diluted, paved film, with transmission electron microscope and X-ray diffraction analysis, can find that the layered silicate lamella in the serous coat of emulsion nano composite acrylic acid copolymerization slurry exists with nano-scale size, prove that above-mentioned prepared emulsion nano composite acrylic acid copolymerization slurry A, B and C are nano composite acrylic acid copolymerization slurry.
Claims (3)
1. weave by a preparation method for emulsification slurry, it is characterized in that being composited by acrylic acid copolymerization slurry and inorganic materials on nano-grade size, its solid content is 10-50%; Wherein said inorganic materials is clay, and its clay content accounts for the 1-30% of acrylic acid copolymerization slurry butt weight; The mix monomer that said acrylic acid copolymerization slurry is made up of two or more third vinyl monomer or vinyl monomer is that solvent is reacted by emulsion copolymerization and prepares with water; The third described vinyl monomer or vinyl monomer comprise vinylformic acid, acrylamide, vinyl cyanide, vinyl acetate, methyl acrylate, ethyl propenoate, butyl acrylate, methacrylic acid, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, vinylbenzene.
2. a kind of weaving according to claim 1 uses the preparation method of emulsification slurry, and it is characterized in that implementing in the steps below: first take clay and be added to the water, adjust ph is 6-9, stirs and makes clay form uniform dispersion liquid, take oil-soluble monomer configuration oil soluble mixed monomer solution again, and take water-soluble monomer and be added to the water dissolving, be 3-7 by alkali adjust ph, obtain water-soluble mixed monomer solution, then in clay dispersion, add the oil soluble mixed monomer solution of 10-50% and the water-soluble mixed monomer solution of 10-50% respectively, add the initiator of the emulsifying agent of the 0.5-5% of water-soluble monomer and oil-soluble monomer total amount and the 0.1-2.5% of water-soluble monomer and oil-soluble monomer total amount again, stir, be warming up to 30-85 DEG C and cause copolyreaction, when in reaction solution, mix monomer reacts completely, start to drip surplus oil dissolubility mix monomer and water-soluble monomer mixing solutions respectively simultaneously, dripped within 3 hours, at 30-85 DEG C, insulation reaction is complete to mix monomer primitive reaction, be warming up to 90-95 DEG C, continue reaction to monomer-free to reflux, be cooled to less than 50 DEG C, adjust ph is 5-7, filter, obtain emulsion nano composite acrylic acid copolymerization slurry.
3. the preparation method of weaving emulsification slurry according to claim 1, is characterized in that described clay is sodium bentonite or sodium-based montmorillonite or kaolin or halloysite; Described initiator is persulphate, comprises ammonium persulphate or Potassium Persulphate, or the redox initiator that persulphate forms with sodium bisulfite or S-WAT; Described oil soluble mixed monomer solution comprises one or more monomers composition in monomer vinyl acetate, methyl acrylate, ethyl propenoate, butyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, vinylbenzene; Described water-soluble mix monomer comprises one or more monomers composition in vinylformic acid, acrylamide, vinyl cyanide, methacrylic acid; Described emulsifying agent refers to by one or both in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, polyoxyethylene nonylphenol ether or two or morely to form.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310653151.2A CN104693343A (en) | 2013-12-06 | 2013-12-06 | Preparation method of emulsification slurry used for weaving |
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| CN201310653151.2A CN104693343A (en) | 2013-12-06 | 2013-12-06 | Preparation method of emulsification slurry used for weaving |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040438A (en) * | 2015-06-26 | 2015-11-11 | 苏州工业园区天意达化学技术有限公司 | Water-based slurry for textile and preparation method thereof |
| CN106480733A (en) * | 2016-11-18 | 2017-03-08 | 无锡明盛纺织机械有限公司 | A kind of polyacrylic spinning sizing agent |
| CN109457479A (en) * | 2018-09-30 | 2019-03-12 | 浙江佳润新材料有限公司 | A kind of slurry and preparation method thereof for luggage |
| CN110512424A (en) * | 2019-08-23 | 2019-11-29 | 广州市迅宏粘合剂有限公司 | A kind of water soluble adhesive and preparation method thereof and its application |
-
2013
- 2013-12-06 CN CN201310653151.2A patent/CN104693343A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040438A (en) * | 2015-06-26 | 2015-11-11 | 苏州工业园区天意达化学技术有限公司 | Water-based slurry for textile and preparation method thereof |
| CN106480733A (en) * | 2016-11-18 | 2017-03-08 | 无锡明盛纺织机械有限公司 | A kind of polyacrylic spinning sizing agent |
| CN109457479A (en) * | 2018-09-30 | 2019-03-12 | 浙江佳润新材料有限公司 | A kind of slurry and preparation method thereof for luggage |
| CN110512424A (en) * | 2019-08-23 | 2019-11-29 | 广州市迅宏粘合剂有限公司 | A kind of water soluble adhesive and preparation method thereof and its application |
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Application publication date: 20150610 |