CN103691335B - A kind of manufacture method of continous way aqueous epoxy emulsion - Google Patents
A kind of manufacture method of continous way aqueous epoxy emulsion Download PDFInfo
- Publication number
- CN103691335B CN103691335B CN201310569861.7A CN201310569861A CN103691335B CN 103691335 B CN103691335 B CN 103691335B CN 201310569861 A CN201310569861 A CN 201310569861A CN 103691335 B CN103691335 B CN 103691335B
- Authority
- CN
- China
- Prior art keywords
- phase
- emulsification
- static mixer
- oil phase
- storage tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to a kind of manufacture method of continous way aqueous epoxy emulsion, the method is by static mixer and the coupling of pipeline high speed shear emulsifying homogeneous machine, make material can carry out pre-emulsification in static mixer, after water oil two fully mixes, again through high speed shear emulsifying homogeneous machine, in the emulsification chamber of homogenizer, material is disperseed uniformly, emulsification, emulsion particle diameter homogenization.This continuous production device provided by the invention, has the features such as treating capacity is large, energy consumption is little, equipment heating amount is little, emulsion particle diameter uniform, controllable, constant product quality.The epoxy resin solution of whole technological process of the present invention and deionized water conveying have been come by screw pump and water pump respectively, and whole production process is carried out at a certain temperature simultaneously.In the process of conveying, carry out heat exchange in order to reducing material with the external world, all pipelines all have employed jacket heat-preservation measure.
Description
Technical field
The present invention relates to the manufacture method of aqueous epoxy emulsion, specifically, is the manufacture method about continous way aqueous epoxy emulsion.
Background technology
The main feature of aqueous epoxide resin paint is that antiseptic property is excellent, and have that low VOC content, smell are less, use safety and the feature such as to can wash by water. therefore, aqueous epoxide resin paint is except for except car paint, although also can be used for metal can coatings and the field such as electrical equipment, medicine equipment. its cost of material is higher, but along with continuous maturation and the development of production technology, aqueous epoxide resin paint will get more and more in industry and coml purposes.
Aqueous epoxy emulsion is the primary raw material of aqueous epoxide resin paint.Current water-borne modification of epoxy resin mainly adopts phase inversion.Phase inversion is that one prepares macromolecule resin emulsion comparatively effective method, almost all macromolecule resins can be obtained corresponding emulsion by means of the effect of additional emulsifying agent by the method for physics emulsification.The process that continuous phase in the former finger multicomponent system of phase reversal transforms under certain condition mutually, as in oil/water/emulsifier system, when continuous phase is changed to oil phase (or from oil phase to aqueous phase) by aqueous phase, in continuous phase limited proportionality, the interfacial tension of system is minimum, and thus the size of decentralized photo is less.Be emulsion by phase inversion by macromolecule resin emulsification, the average grain diameter of its decentralized photo is generally 1 ~ 2 μm.The influence factor of this method is also more, except the equipment that efficient high speed shear must be had to disperse, the type of emulsifying agent, molecular mass size, working concentration and operating temperature etc., in fact all have direct impact to inversion process, size controlling and dispersion and emulsion effect.Recently have people to be studied its inversion process rheological behaviour and phase development, near contrary turning point, the interfacial tension of system profit phase is minimum, and the emulsion now produced has minimum dispersed phase size.And emulsification manufacturing process employing conventional at present is that batch (-type) list still is produced, this production technology can not solve under high shear conditions., water-oil phase mass-and heat-transfer problem, therefore, as the epoxy resin diameter of particle of decentralized photo is comparatively large and domain size distribution is wider in gained emulsion, shape is also irregular, and stability of emulsion and film forming are relatively poor.Existing emulsifying device has all polymorphic types, and the mode of such as batch production has disc type high shear dispersion machine, colloid mill, emulsifying homogeneous machine etc.The feature of this kind equipment is by a phase or multiple Entropy density deviation in another continuous phase, and under normal conditions, these two is immiscible mutually.This kind equipment is in the process of emulsify at a high speed epoxy resin, there is obvious defect, in process due to the Phase inversion emulsification of epoxy resin, viscosity can sharply rise, form a kind of thick liquid without mobility, therefore in emulsion process, a large amount of kinetic transformation is formed by dispersing apparatus and next heat well can not be conducted by material, the temperature of charge causing dispersion impeller periphery sharply rises, have impact on the efficiency of surfactant, the heat simultaneously gathered causes the temperature at center of turntable place very high, causes equipment to cross quick-wearing.
What can be used as continous way production has pipeline high shear homogeneous emulsifying machine, static mixer etc.Static mixer is a kind of high-efficiency mixing device not having moving component, the mixed process of static mixer is undertaken by the hybrid element be fixed in pipe, due to the effect of hybrid element, make fluid constantly change flow direction, thus reach the effect of emulsification pretreatment.Pipeline-type emulsifying machine operation principle is basic identical with common high-shear emulsion machine, is all the sophisticated design by rotor, produces powerful shearing force to realize the object of mixing, pulverizing, emulsification in High Rotation Speed.But the maximum difference of pipeline-type emulsifying machine is that it can configure one or more sets rotors; can also be connected with static mixer simultaneously; realize continuous seepage; one endfeed; one end discharging; the heat that dispersing shear is formed not easily is assembled, and also stabilizes the quality of product while proterctive equipment, and production efficiency have also been obtained and promotes greatly in addition.
Summary of the invention
The object of the invention is for deficiency of the prior art, a kind of manufacture method of continous way aqueous epoxy emulsion is provided.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of manufacture method of continous way aqueous epoxy emulsion, the concrete steps of described method are as follows: adopt oil phase pump (M1) and aqueous phase pump (M2) respectively the deionized water two-phase in the epoxy resin solution containing surfactant in oil phase storage tank (A) and aqueous phase storage tank (B) to be pressed certain mass proportion requirement and send in static mixer (C), the flow of oil phase is 3-5KG/min, the flow of aqueous phase is 0.3-0.6L/min, after static mixer (C), the emulsification chamber of pipeline high speed shear emulsifying homogeneous machine (D) is entered in pumping again, by the High Rotation Speed of emulsification chamber rotor, water-oil phase is by further emulsification and homogenization, and the phase inversion point through pipeline high speed shear emulsifying homogeneous machine (D) exit detects conductivity meter (F), be shown as oil-in-water mutually after, material is transported in thinning tank (E), then interpolation deionized water is diluted to quality solid content is 52%, obtain final products, otherwise be pumped to static mixer front end and repeat emulsion process, be 5-10:1 containing the deionized water two-phase mass ratio in the epoxy resin solution of surfactant and aqueous phase storage tank (B) in described oil phase storage tank (A), the rotating speed of the High Rotation Speed of emulsification chamber rotor is 500-3000rpm.
The described epoxy resin solution containing surfactant is obtained by following method: in advance in oil phase storage tank in (A), and solid epoxy and cosolvent and surfactant being heated is dissolved into solution state.
Described cosolvent is propylene glycol monomethyl ether.
Described surfactant is APES.
The invention has the advantages that:
1, the invention provides a kind of manufacture method of continous way aqueous epoxy emulsion, the method is by static mixer and the coupling of pipeline high speed shear emulsifying homogeneous machine, make material can carry out pre-emulsification in static mixer, after water oil two fully mixes, again through high speed shear emulsifying homogeneous machine, in the emulsification chamber of homogenizer, material is disperseed uniformly, emulsification, emulsion particle diameter homogenization.This continuous production device provided by the invention, has the features such as treating capacity is large, energy consumption is little, equipment heating amount is little, emulsion particle diameter uniform, controllable, constant product quality.
2, the device adopted in this method includes static mixer and the pipeline high speed shear emulsifying homogeneous machine of band insulation jacket, and Flange joint is passed through in the outlet of static mixer and the import of pipeline high speed shear homogeneous emulsifying machine.
3, whether oil-in-water state has been turned to from Water-In-Oil for detecting emulsion in the present invention, conductivity probe is provided with in the exit of pipeline high speed shear emulsifying homogeneous machine, when electrical conductivity is raised to deionization electrical conductivity of water by 0, prove that this process occurs, subsequent operation can be carried out, otherwise, another road valve in exit will be opened, material is led back emulsification again before static mixer by other pipe.
4, the epoxy resin solution of whole technological process of the present invention and deionized water conveying have been come by screw pump and water pump respectively, and whole production process is carried out at a certain temperature simultaneously, generally at 40-85 DEG C, is preferably 65-75 DEG C.In the process of conveying, carry out heat exchange in order to reducing material with the external world, all pipelines all have employed jacket heat-preservation measure.
5, the present invention is compared with traditional batch (-type) emulsifying process, when reaching equal emulsifying effectiveness, greatly can reduce floor space, having saved equipment investment, and the ability of emulsification strengthens greatly, can reach 1-3 ton/hour.
6, devise static mixer at emulsify at a high speed shear and homogenize machine leading portion, epoxy resin, deionized water and surfactant are fully mixed before entering homogenizer, the pipeline section that static mixer is 30 centimeters by two segment length forms, and has Flange joint between each section.Can pre-emulsification be realized through static mixer, ensure that the quality of emulsification.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation adopting continuous emulsifying aqueous epoxy emulsion device provided by the invention.
Accompanying drawing 2 records average grain diameter schematic diagram for the embodiment of the present invention 2.
Detailed description of the invention
Below in conjunction with accompanying drawing, detailed description of the invention provided by the invention is elaborated.
Embodiment 1
Fig. 1 is the structural representation adopting continuous emulsifying aqueous epoxy emulsion device provided by the invention.As shown in Figure 1, this device includes oil phase storage tank (A), aqueous phase storage tank (B) and thinning tank (E, thinning tank is again product storage tank or dilution still).Static mixer (C) and pipeline high speed shear emulsifying homogeneous machine (D) of emulsion dispersion effect has also been comprised in addition in device.All devices connects by the pipeline of band insulation jacket.
In oil phase storage tank (A), solid epoxy and a small amount of cosolvent and surfactant are heated after being dissolved into solution state, be pumped to static mixer (C) through M1 oil phase, open aqueous phase storage tank (B) simultaneously, deionization is passed through M2 aqueous phase transport pump to static mixer (C).Flow controls by flowmeter, and M1 flowmeter adopts mass flowmenter, and M2 adopts volume flowmeter.Under normal circumstances, profit charge proportion will strictly control, and preferred proportion is 5-10:1(weight ratio).When oil mixing with water material is through static mixer (C) pre-emulsification, be thoroughly mixed evenly and enter pipeline high speed shear emulsifying homogeneous machine (D).Phase inversion point is set in the exit of (D) of pipeline high speed shear emulsifying homogeneous machine and detects conductivity meter (F), be pumped to thinning tank (E) after phase inversion, be diluted to solids content 52% by deionized water, obtain final products.The stability property figureofmerit of epoxy resin latex meets (1) dewatering ability: 2000 revs/min, 30 minutes not stratified (2) storage stabilities: 6 months emulsion not breakdown of emulsion layering (3) average grain diameter: < 1.5 μm.
Embodiment 2
In (A), 601 epoxy resin of 95.8KG, the propylene glycol monomethyl ether of 15.4KG and the APES of 11.8KG is added in advance in oil phase storage tank.Heating for dissolving obtains epoxy solution.Adopt continuous emulsifying technological process as shown in Figure 1, with oil phase pump (M1) and aqueous phase pump (M2) respectively by the water in the epoxy solution in oil phase tank (A) and aqueous phase tank (B) according to 6.8:1(mass ratio) ratio send in static mixer (C), the flow of oil phase is 3kg/min, and the flow of aqueous phase is 0.45L/min.After the pre-dispersed emulsification of static mixer, enter pipeline high speed shear emulsifying homogeneous machine (D), high-speed shearing machine rotating speed is arranged on 2000rpm.Now recording cutter exit electrical conductivity is 20us/cm.Display epoxy solution phase inversion is oil-in-water state.Phase inversion afterproduct is pumped to thinning tank (E), is diluted to by deionized water the white " milky " liquid that quality solid content is 52%.(utilizing laser particle size analyzer device to detect) now records average grain diameter D
90be 0.873 μm (Fig. 2).
It should be noted that: whole process is continuous process from charging, emulsification, discharging, the conveying of material all has pump and mass flowmenter to control, and usual material only need be heated to 40-85 DEG C, and preferable temperature is at 65-75 DEG C.The common manufacturing capacity of this technique is 1-3 ton per hour.
Embodiment 3
In (A), 601 epoxy resin of 95.8KG, the propylene glycol monomethyl ether of 15.4KG and the APES of 11.8KG is added in advance in oil phase storage tank.Heating for dissolving obtains epoxy solution.Adopt continuous emulsifying technological process as shown in Figure 1, with oil phase pump (M1) and aqueous phase pump (M2) respectively by the water in the epoxy solution in oil phase tank (A) and aqueous phase tank (B) according to 8:1(mass ratio) ratio send in static mixer (C), the flow of oil phase is 3.5kg/min, and the flow of aqueous phase is 0.35L/min.After the pre-dispersed emulsification of static mixer, enter pipeline high speed shear emulsifying homogeneous machine (D), high-speed shearing machine rotating speed is arranged on 1000rpm.Now recording cutter exit electrical conductivity is 20us/cm.Display epoxy solution phase inversion is oil-in-water state.Phase inversion afterproduct is pumped to thinning tank (E), is diluted to by deionized water the white " milky " liquid that quality solid content is 52%.Now record average grain diameter D
90it is 0.871 μm.
Embodiment 4
In (A), 601 epoxy resin of 95.8KG, the propylene glycol monomethyl ether of 15.4KG and the APES of 11.8KG is added in advance in oil phase storage tank.Heating for dissolving obtains epoxy solution.Adopt continuous emulsifying technological process as shown in Figure 1, with oil phase pump (M1) and aqueous phase pump (M2) respectively by the water in the epoxy solution in oil phase tank (A) and aqueous phase tank (B) according to 10:1(mass ratio) ratio send in static mixer (C), the flow of oil phase is 5kg/min, and the flow of aqueous phase is 0.6L/min.After the pre-dispersed emulsification of static mixer, enter pipeline high speed shear emulsifying homogeneous machine (D), high-speed shearing machine rotating speed is arranged on 500rpm.Now recording cutter exit electrical conductivity is 20us/cm.Display epoxy solution phase inversion is oil-in-water state.Phase inversion afterproduct is pumped to thinning tank (E), is diluted to by deionized water the white " milky " liquid that quality solid content is 52%.Now record average grain diameter D
90it is 0.852 μm.
Embodiment 5
In advance in oil phase storage tank in (A), add 601 epoxy resin of 95.8KG, the propylene glycol monomethyl ether of 15.4KG and the APES of 11.8KG, heating for dissolving obtains epoxy solution.
Adopt continuous emulsifying technological process as shown in Figure 1, with oil phase pump (M1) and aqueous phase pump (M2) respectively by the water in the epoxy solution in oil phase tank (A) and aqueous phase tank (B) according to 5:1(mass ratio) ratio send in static mixer (C), the flow of oil phase is 4kg/min, and the flow of aqueous phase is 0.45L/min.After the pre-dispersed emulsification of static mixer, enter pipeline high speed shear emulsifying homogeneous machine (D), high-speed shearing machine rotating speed is arranged on 3000rpm.Now recording cutter exit electrical conductivity is 20us/cm.Display epoxy solution phase inversion is oil-in-water state.Phase inversion afterproduct is pumped to thinning tank (E), is diluted to by deionized water the white " milky " liquid that quality solid content is 52%.Now record average grain diameter D
90it is 0.952 μm.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the inventive method; can also make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.
Claims (1)
1. the manufacture method of a continous way aqueous epoxy emulsion, it is characterized in that, the concrete steps of described method are as follows: adopt oil phase pump (M1) and aqueous phase pump (M2) respectively the deionized water two-phase in the epoxy resin solution containing surfactant in oil phase storage tank (A) and aqueous phase storage tank (B) to be pressed certain mass proportion requirement and send in static mixer (C), the flow of oil phase is 3-5KG/min, the flow of aqueous phase is 0.3-0.6L/min, after static mixer (C), the emulsification chamber of pipeline high speed shear emulsifying homogeneous machine (D) is entered in pumping again, by the High Rotation Speed of emulsification chamber rotor, water-oil phase is by further emulsification and homogenization, and the phase inversion point through pipeline high speed shear emulsifying homogeneous machine (D) exit detects conductivity meter (F), be shown as oil-in-water mutually after, material is transported in thinning tank (E), then interpolation deionized water is diluted to quality solid content is 52%, obtain final products, otherwise be pumped to static mixer front end and repeat emulsion process, be 5-10:1 containing the deionized water two-phase mass ratio in the epoxy resin solution of surfactant and aqueous phase storage tank (B) in described oil phase storage tank (A), the rotating speed of the High Rotation Speed of emulsification chamber rotor is 500-3000rpm, the described epoxy resin solution containing surfactant is obtained by following method: in advance in oil phase storage tank (A), and solid epoxy and cosolvent and surfactant being heated is dissolved into solution state, described cosolvent is propylene glycol monomethyl ether, described surfactant is APES.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310569861.7A CN103691335B (en) | 2013-11-13 | 2013-11-13 | A kind of manufacture method of continous way aqueous epoxy emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310569861.7A CN103691335B (en) | 2013-11-13 | 2013-11-13 | A kind of manufacture method of continous way aqueous epoxy emulsion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103691335A CN103691335A (en) | 2014-04-02 |
| CN103691335B true CN103691335B (en) | 2016-02-24 |
Family
ID=50353095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310569861.7A Active CN103691335B (en) | 2013-11-13 | 2013-11-13 | A kind of manufacture method of continous way aqueous epoxy emulsion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103691335B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084330B (en) * | 2017-12-27 | 2020-07-03 | 佛山市飞吸高分子材料科技有限公司 | Preparation method of acrylic ester porous polymer |
| CN110935733B (en) * | 2018-09-21 | 2021-08-17 | 宝山钢铁股份有限公司 | Emulsion particle size online control method and system |
| CN109908778A (en) * | 2019-03-18 | 2019-06-21 | 肇庆力合技术发展有限公司 | A kind of device and method of continuous production emulsion |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101601977A (en) * | 2009-07-10 | 2009-12-16 | 葛洲坝易普力股份有限公司 | Method for preparing emulsion matrix safely and efficiently |
-
2013
- 2013-11-13 CN CN201310569861.7A patent/CN103691335B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101601977A (en) * | 2009-07-10 | 2009-12-16 | 葛洲坝易普力股份有限公司 | Method for preparing emulsion matrix safely and efficiently |
Non-Patent Citations (1)
| Title |
|---|
| 水性环氧乳液稳定性研究及分析;刘颖等;《玻璃纤维》;20071231(第2期);第1-4、9页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103691335A (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5046856A (en) | Apparatus and method for mixing fluids | |
| JP5795794B2 (en) | Emulsifying device for continuous production of emulsion and / or dispersion | |
| US7581872B2 (en) | Gel mixing system | |
| CN207392003U (en) | A kind of modified pitch production system | |
| CN103691335B (en) | A kind of manufacture method of continous way aqueous epoxy emulsion | |
| US8641266B2 (en) | Horizontal-flow hydration apparatus | |
| CN202490592U (en) | Powder and liquid mixing device | |
| US20040218463A1 (en) | Gel mixing system | |
| CN209519696U (en) | A kind of suspending agent production system of high fineness | |
| CN103349937B (en) | A kind of continuous emulsification device | |
| CN102794118B (en) | Method and device for high efficiency preparation of oil-displacement polymer used for oil field | |
| CN209652197U (en) | A kind of combination unit preparing emulsified bases | |
| CN103070164A (en) | Novel method for preparing pesticide suspending agents | |
| CN204365156U (en) | Automatic matching device for emulsion | |
| CN1340375A (en) | High-shear emulsifying homogenizer | |
| CN208517303U (en) | A kind of emulsion static emulsion equipment | |
| CN204891619U (en) | Polymer evenly dissolves fast, bubble -free curing system | |
| CN203291730U (en) | Powder mixing and emulsification device | |
| CN202700420U (en) | Emulsifying device | |
| CN205152155U (en) | Emulsified asphalt device | |
| CN217646220U (en) | Superhigh speed emulsification pump | |
| CN204699653U (en) | Acrylonitrile-butadiene-styrene copolymer additive mixing device | |
| Scott et al. | A practical guide to equipment selection and operating techniques | |
| CN213556401U (en) | Water-based resin circulation emulsification device | |
| CN204247083U (en) | A kind of emulsifier unit |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 200331 Gulang Road, Shanghai, No. second, building 1167, No. Patentee after: Shanghai Huayi Fine Chemical Co., Ltd. Shanghai Xinhua resin factory Address before: 200331 No. 1167, Gulang Road, Shanghai, Putuo District Patentee before: Shanghai Changfeng Chemical Industrial Factory of Shanghai Xinhua Resin Co., Ltd. |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20170327 Address after: 200020 Shaanxi South Road, Shanghai, No. 345 Patentee after: SHANGHAI HUAYI FINE CHEMICAL CO., LTD. Address before: 200331 Gulang Road, Shanghai, No. second, building 1167, No. Patentee before: Shanghai Huayi Fine Chemical Co., Ltd. Shanghai Xinhua resin factory |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200730 Address after: 201512 Huadao 707, Jinshan District, Shanghai Patentee after: SHANGHAI HUAYI PAINT Co.,Ltd. Address before: 200020 Shaanxi South Road, Shanghai, No. 345 Patentee before: SHANGHAI HUAYI FINE CHEMICAL Co.,Ltd. |
|
| TR01 | Transfer of patent right |