CN205205064U - Device of super two thin coating of production that modified particle was decoratied - Google Patents
Device of super two thin coating of production that modified particle was decoratied Download PDFInfo
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- CN205205064U CN205205064U CN201520955979.8U CN201520955979U CN205205064U CN 205205064 U CN205205064 U CN 205205064U CN 201520955979 U CN201520955979 U CN 201520955979U CN 205205064 U CN205205064 U CN 205205064U
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Abstract
The utility model discloses a device of super two thin coating of production that modified particle was decoratied. The device includes the device is including super two thin coating composition A production systems and super two thin coating composition B production systems, super two thin coating composition A production system includes first subsystem and second subsystem, first subsystem is including modified particle high speed dispersion machine, the parallelly connected reaction unit of modified six cauldrons on the particle and hydrocyclone, the second subsystem includes resin monomer raw materials premixer, six cauldron series connection reaction unit of fluorine -containing hydroxy acrylic resin and resin solvent pre -heater, super two thin coating composition B production system includes the two cauldron series connection reaction unit of fluorine -containing PU performed polymer curing agent, performed polymer raw material mixing ware and performed polymer feed preheater, the utility model discloses the device can realize that continuous production, easy maintenance, exploitativeness are good, the utility model discloses the simple process that the method adopted.
Description
Technical field
The utility model relates to the field of super two thin coating, is specifically related to the device of the super two thin coating of production that a kind of modified particle is modified.
Background technology
Super two open coat is with a wide range of applications in daily life with in national product because of the characteristic of its hydrophobic oleophobic, especially the super two thin coating of the environment-friendly double-component be mixed with by surface treated silicon-dioxide micro-and nano-particles and fluorine resin, the effect such as its automatically cleaning, protection against corrosion, anti-freeze wax deposition, anti-adhesion makes it be widely used in the lives such as building materials, petroleum pipe line, glass-ceramic, leather, electronic product, kitchen guarding's apparatus and production.
In recent years, a lot of researchist and team are all studied the production of super two thin coating, and obtain good achievement in research.A lot of research about super two thin coating at present can obtain international accreditation, but super two thin coating does not but realize large-scale industrial production, reason also there are some basic problems about the production of super two thin coating: 1. in performance: when super two thin coating comes into operation, be easy to and formation gap, interface, the problem such as cause coating oxidation, come off, shortens its work-ing life;
the complex manufacturing of super two thin coating, the general production cycle is long, is difficult to realize continuous seepage, and cause its production efficiency low, production cost is high;
adaptability: use electrochemical deposition method to produce super two open coat and be only applicable to specific surface, use range is narrow.
The super two thin material good for processability and make up above-mentioned basic problem, the utility model proposes with SiO
2micro-and nano-particles, multiple Acrylic Acid Monomer (MMA, BA, HAMA), perfluoroalkyl ethanol, HDI tripolymer are raw material, and use the multi-solvents such as N-BUTYL ACETATE, acetone and the auxiliary such as initiator, thinner; Production main products is the super two thin material of the environment-friendly double-component of purity>=99.7%, and impurity is a small amount of isocyanic ester autopolymer, a small amount of reaction monomers of not eliminating mainly, can ignore its impact; This technique is also for counting seldom and the environment-friendly type production system of very high purity.
Utility model content
In order to overcome deficiency and the shortcoming of above-mentioned background technology, the first object of the present utility model is to propose a kind of novel, simply super two thin material produce mode of technique;
This second practical object is the preparation method of the fluorine-containing super two thin coating providing the fluorine-containing Hydroxylated acrylic resin of nano modification and fluorine-containing PU performed polymer to be obtained by crosslinking reaction;
3rd object of the present utility model is the continuity realizing producing;
4th object of the present utility model is the application providing above-mentioned super two thin coating;
The purpose of this utility model realizes mainly through following technical proposals.
A device for the super two thin coating of production that modified particle is modified, described device comprises super two thin coating composition A production system and super two thin coating composition B production system; Described super two thin coating composition A production system comprises the first subsystem and the second subsystem;
Described first subsystem comprises modified particle high speed dispersor, modified particle six still reaction unit in parallel and wet cyclone; Described second subsystem comprises resin monomer raw material premixer, fluorine-containing Hydroxylated acrylic resin six still cascade reaction device and resin solvent preheater; Described super two thin coating composition B production system comprises fluorine-containing PU performed polymer solidifying agent two still cascade reaction device, performed polymer material stirrer and performed polymer feed preheater;
Described first subsystem and the second subsystem are linked together by resin Composition A agitator;
In first subsystem, described modified particle high speed dispersor is connected by pipeline and modified particle six still reaction unit in parallel through pump, and described modified particle six still reaction unit in parallel is connected with wet cyclone by pipeline through pump; Described wet cyclone liquid exit is connected to storage tank before the charging of modified particle high speed dispersor by pipeline, solid outlet is connected to resin Composition A agitator by pipeline; Before the charging of described modified particle high speed dispersor, storage tank is connected with modified particle high speed dispersor by pipeline;
In second subsystem, described resin monomer raw material premixer is connected with fluorine-containing Hydroxylated acrylic resin six still cascade reaction device by pipeline, described resin solvent preheater is connected with fluorine-containing Hydroxylated acrylic resin six still cascade reaction device by pipeline, and described fluorine-containing Hydroxylated acrylic resin six still cascade reaction device is connected with resin Composition A agitator by pipeline through pump;
In super two thin coating composition B production system, described performed polymer feed preheater is connected with performed polymer material stirrer by pipeline, and performed polymer material stirrer is connected by the two still cascade reaction device of pipeline and fluorine-containing PU performed polymer solidifying agent through pump.
Further, described modified particle six still reaction unit in parallel adopts six still parallel forms, greatly can improve the throughput of subsystem 1, facilitate the maintenance of reactor simultaneously.
Further, described fluorine-containing Hydroxylated acrylic resin reaction unit (4) adopts multi-floating bodies reaction formation, and wherein the number of reactor is 4-8, and can make up in traditional coating production technique to rely on increases reaction kettle body sum quantity to improve the shortcoming of turnout.
A method for the super two thin coating of production that modified particle is modified, comprises the steps:
(1) preparation of the micron particle of modification: ten difluoro heptyl propyl trimethoxy silicanes and micron particle Al
2o
3with nanoparticle SiO
2there is the micro-nano particle that linked reaction obtains modification; Described linked reaction is using ten difluoro heptyl propyl trimethoxy silicanes as coupling agent;
(2) preparation of super two thin coating composition A: the micro-nano particle of modification step (1) obtained joins in fluorine-containing Hydroxylated acrylic resin, add dispersion agent again, flow agent and defoamer, high-speed stirring 27 ~ 35min, high speed dispersion 27 ~ 35min, high-speed stirring 27 ~ 35min again, obtains modification micro-nano particle and modifies fluorine-containing Hydroxylated acrylic resin, i.e. super two thin coating composition A;
(3) preparation of super two thin coating composition B: HDI tripolymer and solid perfluoroalkyl ethanol are pressed (2.7 ~ 3.2): 1 proportioning polymerization reaction take place obtains fluorine-containing PU performed polymer, i.e. super two thin coating composition B;
(4) described super two thin coating is the super two thin coating of two-pack, stores respectively before using; According to super two thin coating composition A during use: super two thin coating composition B=(2 ~ 3): the ratio of 1 mixes, and can use.
In aforesaid method, in step (1), the solvent of described linked reaction is ethanol, and the massfraction of described solvent is 76.88% ~ 78.76%; The modified additive of described linked reaction is acetone, and described modified additive massfraction is 4.02% ~ 4.55%; The pH scope of described linked reaction is 3.5 ~ 4.5, and buffer reagent used is acetic acid; Micron particle Al in described linked reaction
2o
3with nanoparticle SiO
2it is the modification micro-nano particle prepared by sol-gel method (Sol-gel); Modification micro-nano particle is needed to mix with coupling agent ten difluoro heptyl propyl trimethoxy silicane in described coupling reaction process, rear ultrasonic disperse 0.5h, reheat, return stirring 5 ~ 7 hours, cooling centrifugation, finally dries complete the modification micro-nano particle of finishing.
In aforesaid method, in step (2), micro-nano particle and the fluorine-containing Hydroxylated acrylic resin add-on of described modification meet: the mass ratio of fluorine-containing Hydroxylated acrylic resin and modification micro-nano particle is (1.6 ~ 2): 1.
In aforesaid method, the composition of described dispersion agent is the acrylic ester polymer of cation group, and solvent is propylene glycol monomethyl ether monoacetate or dimethylbenzene; Described flow agent is vinylformic acid flow agent or modified acroleic acid flow agent, and wherein modification flow agent is fluorine richness or phosphate modified flow agent; Described defoamer is polyether-modified type silicone antifoam agent.
In aforesaid method, described fluorine-containing Hydroxylated acrylic resin is polymerized by multiple Acrylic Acid Monomer and fluorochemical monomer; Described multiple Acrylic Acid Monomer comprises methyl methacrylate (MMA), butyl acrylate (BA) hydroxyethyl methylacrylate (HEMA), and wherein point monomer weight ratio is MMA:BA:HEMA=(1.6 ~ 2): (1.1 ~ 1.3): 1; Described fluorochemical monomer is methacrylic acid ten trifluoro monooctyl ester, and this fluorine monomer adopts the mode of dropping to add in reaction process, and this monomer accounts for 30% ~ 33% of monomer total mass.
In aforesaid method, the insulating process of described polyreaction completes respectively in 6 stills; Described 6 stills are series arrangement, and in each still, the reaction times is 50min, and temperature is 85 DEG C ~ 95 DEG C; Still connects water trap simultaneously, removes wherein moisture by condensing reflux.
Aforesaid method comprises the steps:
Modified particle high speed dispersor is entered into from storage tank using as the ethanol of solvent and acetone; Raw material ten diheptyl propyl trimethoxy silicane enters the particle modified high speed dispersor of micro-nano from head tank simultaneously; Add vinegar acid for adjusting pH large most 3.5 ~ 4.5; Be uniformly mixed fully, enter into preheater through mixing material pump, enter into modified particle six still reaction unit in parallel after preheating, add micron particle Al simultaneously
2o
3nanoparticle SiO
2=(0.3 ~ 0.5): 1, reflux continues 5 ~ 7 hours, mixed solution after reflux arrives wet cyclone by pump after first being cooled by condenser, the micro-nano particle of the surface modification obtained is transferred to dryer from lower port, dehydration 2 ~ 4h is carried out at 110 DEG C ~ 130 DEG C, obtain the micro-nano particle of dry surface modification, be stored in storage tank for subsequent use;
Solvent butyl acetate and methyl iso-butyl ketone (MIBK) are mixed into storage tank, put in fluorine-containing Hydroxylated acrylic resin six still cascade reaction device after resin solvent preheater preheats is to 92 DEG C ~ 97 DEG C;
Raw material methyl methacrylate, butyl acrylate, hydroxyethyl methylacrylate, N-BUTYL ACETATE and initiator enter into resin monomer raw material premixer from head tank respectively, obtain mixed solvent, simultaneously add mixed solvent wherein, final fluorine-containing Hydroxylated acrylic resin; Through fluorine-containing Hydroxylated acrylic resin pump, fluorine-containing Hydroxylated acrylic resin is extracted out from fluorine-containing Hydroxylated acrylic resin six still cascade reaction device, transfer in monomer separation device, reflux dewatering, transfers to resin Composition A agitator by fluorine-containing Hydroxylated acrylic resin pump, for subsequent use;
By fluorine-containing Hydroxylated acrylic resin by configurator by fluorine-containing Hydroxylated acrylic resin: modification micro-nano particle=(1.6 ~ 2) of surface modification: 1 continues to add modification micro-nano particle in resin Composition A agitator, high-speed stirring, high speed dispersion, high-speed stirring again, must super two thin coating composition A;
Fluorine-containing PU performed polymer solidifying agent production process: solvent butyl acetate and hexone join mixing agitator from head tank, stir, join in fluorine-containing PU performed polymer material stirrer after arriving the heating of performed polymer raw material mixed solvent preheater by mixing solutions pump, solid perfluoroalkyl ethanol is joined in fluorine-containing PU performed polymer material stirrer simultaneously; After solids all dissolve, utilize flasher to remove moisture, obtain mixed solution 1;
First mixed solution 1 is added the two still cascade reaction device of fluorine-containing PU performed polymer solidifying agent, then add mixed solution 2 by the header tank that configurator is housed; Described mixed solution 2 is the mixing solutions of dibutyl tin dilaurate and HDI tripolymer and N-BUTYL ACETATE; Reaction insulation 2.2h-3.1h, temperature of reaction is 85 DEG C ~ 90 DEG C, then stops heating after continuing to stir 25min-32min, is cooled to room temperature, must super two thin coating composition B.
In aforesaid method, described Acrylic Acid Monomer is easy to self-polymeric reaction occurs, and needs to add stopper, need to carry out pre-treatment to Acrylic Acid Monomer before production in storage process.Described stopper is quinhydrones (Isosorbide-5-Nitrae-Resorcinol); Described polyreaction needs benzoyl peroxide (BPO) as initiator, and initiator amount is 0.8% ~ 1.85% of total quality of material; In described polyreaction, solvent for use is N-BUTYL ACETATE and methyl iso-butyl ketone (MIBK) (N-BUTYL ACETATE: methyl iso-butyl ketone (MIBK)=(4.2 ~ 4.6): 1); 5h need be incubated under 85 DEG C ~ 95 DEG C conditions in described polymerization process; Described polyreaction insulating process completes, respectively see Fig. 2 in 6 stills; Described fluorine-containing Hydroxylated acrylic resin need can enter next unit through reflux dewatering removal of impurities; Described reflux dewatering, the water ratio as solvent is bigger than normal, after dropping into solvent, before mix monomer dropwise reaction, should ensure time enough, under return stirring, dewater to solvent, till water is purified.Reaction is after the later stage adds whole solvent, technique requires more backflow 30 minutes, this technique be can not ignore, and one guarantees that system moisture is all taken out of by backflow, it two guarantees that system residual monomer/initiator is few, in order to avoid cause the appearance of the problems such as resin smell is large, painting weather resistance variation.Described HDI tripolymer is hexamethylene diisocyanate trimer, belongs to isocyanates, in HDI tripolymer, have cumulative double bond, and chemical property is very active, and the compound containing reactive hydrogen such as Yi Yushui, alcohol, phenol and amine reacts; Described solid perfluoroalkyl ethanol is 12.8% ~ 13.32% of total quality of material.The solvent of described reaction is N-BUTYL ACETATE and hexone (N-BUTYL ACETATE: hexone=(4.2 ~ 4.9): 1); Described reaction used catalyst is dibutyl and tin laurate; Be incubated 2.5h in described reaction process, between the strict control reaction period, still temperature is between 85 ~ 90 DEG C, and adjust flux makes HDI tripolymer add in 2h, then stops heating after continuing to stir 30min, allows solution be cooled to room temperature; The basis for estimation of described reaction end measures free-NCO groups content in still, when free-NCO content is lower than 8%, represents that reaction terminates; Described performed polymer building-up reactions also need be carried out in nitrogen environment.
The method of the super two thin coating of production that modified particle is modified, production modification micro-nano particle raw material and quality proportioning thereof are respectively: ten difluoro heptyl propyl trimethoxy silicane 12.27%-13.04%, micron particle 1.46%-1.84%, nanoparticle 2.41%-2.73%, acetone 4.02%-4.55%, ethanol 76.88%-78.76% be about 3-5 by acetic acid adjust ph.
In aforesaid method, raw material and the quality proportioning thereof of producing fluorine-containing Hydroxylated acrylic resin are respectively methacrylic acid ten trifluoro monooctyl ester 11.5%-12.75%, benzoyl peroxide 0.8%-1.85%, hydroxyethyl methylacrylate 5.87%-7.34%, butyl acrylate 6.5%-8.64%, methyl methacrylate 10.8%-12.3%, methyl iso-butyl ketone (MIBK) 10.8%-11.53%, N-BUTYL ACETATE 48.5%-50.2%.
In aforesaid method, produce raw material and quality proportioning hexamethylene diisocyanate trimer 36.2%-36.75%, perfluoroalkyl ethanol 12.8%-13.32%, N-BUTYL ACETATE 39.1%-41.05%, methyl iso-butyl ketone (MIBK) 8.32%-9.31%, the butyl tin dilaurate 0.5%-1.0% respectively thereof of fluorine-containing PU performed polymer.
In aforesaid method, in order to make super two thin material effects material >=99.7% of environment-friendly double-component obtained, each several part proportioning, reaction conditions are clear and definite.Three productive unit materials proportionings all use configurator accurately to carry out.With the addition of pH meter having in the operation of requirement potential of hydrogen, with acetic acid control ph within the limits prescribed.Mixing agitator, ultrasonic disperse machine, condensing reflux, react fully.Thermally sensitive reaction workshop section, device is arranged in pairs or groups steam heater temperature controlling system, and the way added materials by feed-back regulatory mechanism and segmentation controls temperature of reaction.Finally measure free in still-NCO group content to reach 8% explanation and be reacted to terminal.
The utility model products obtained therefrom and water, oily contact angle are 150 °-170 °; The super two thin purity of gained is high, performance good, can be used for the fields such as micro-fluidic chip design, draft reduction material, the anti-adhesive surface of liquid orientation transport.
The utility model principle: the utility model production process is made up of three parts is micro-nano improving particle surface production process respectively, fluorine-containing Hydroxylated acrylic resin production process and fluorine-containing PU performed polymer solidifying agent production process.Whole production process achieves production serialization.Be dependence six still reaction unit in parallel respectively, limit, the batch production village is continuous seepage by six still cascade reaction devices, two still cascade reaction device.Produce super two thin coating and have employed the method that modification micro-nano particle modifies fluorine-containing Hydroxylated acrylic resin.The introducing of fluorine element reduces the surface energy of coating, enhances grease proofing ability, and modification micro-nano particle increases the roughness of coatingsurface, enhances waterproof ability, makes coating have super two function of dredging.
The utility model and existing Technical comparing, the advantage had and effect as follows:
(1) in device of the present utility model micro-and nano-particles surface modification reaction in quantity of solvent large, the reaction volume of needs is large, and traditional single still production model cannot meet, therefore for realizing downstream continuous discharge, adopts the mode of 6 still parallel connections;
(2) synthesis of the present utility model fluorine-containing Hydroxylated acrylic resin partial reaction overlong time, the mode of 6 still series connection is adopted to guarantee the continuity of producing, reach identical productive rate, only need the reactor of more small volume, smaller amounts, compensate in traditional coating production technique to rely on and increase reaction kettle body sum quantity to improve the shortcoming of productive rate, use manpower and material resources sparingly simultaneously;
(3) the super two thin coating of environment-friendly double-component of purity >=99.7% of main products produced of the utility model, the mainly a small amount of isocyanic ester autopolymer of impurity, a small amount of reaction monomers do not eliminated, but it is very little to the performance impact of product, can ignore;
(4) the utility model is in order to make reactant reaction abundant, adds the auxiliarys such as N-BUTYL ACETATE, acetone equal solvent and initiator, thinner, film coalescence aid, defoamer in production process, realizes high yield, high purity is produced;
(5) the utility model modified Nano particulate specific surface area is large, has strong surface effects, it is scattered in polymkeric substance, is convenient to coupling agent absorption, can Reaction time shorten and improve molecular material performance widely;
(6) the utility model utilizes two still cascade reaction device to synthesize fluorine-containing PU performed polymer, realizes continuous discharge.
Accompanying drawing explanation
Fig. 1 is micro-nano improving particle surface six still reaction unit in parallel;
Fig. 2 is fluorine-containing Hydroxylated acrylic resin six still cascade reaction device;
Fig. 3 is the device of the super two thin coating of production that a kind of modified particle of the utility model is modified;
In figure, all parts is as follows: the particle modified high speed dispersor 1 of micro-nano, micro-nano improving particle surface six still reaction unit 2 in parallel, wet cyclone 3, fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4, resin Composition A agitator 5, the two still cascade reaction device 6 of fluorine-containing PU performed polymer solidifying agent, fluorine-containing PU performed polymer material stirrer 7, performed polymer raw material mixed solvent preheater 8, resin solvent preheater 9, resin monomer raw material premixer 10, reactor I 11, reactor II 12, reactor III 13, reactor IV 14, reactor V 15, reactor VI 16.
Embodiment
With reference to Fig. 1 ~ Fig. 3, the utility model comprises the particle modified high speed dispersor 1 of micro-nano, micro-nano improving particle surface six still reaction unit 2 in parallel, wet cyclone 3, fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4, resin Composition A agitator 5, the two still cascade reaction device 6 of fluorine-containing PU performed polymer solidifying agent, fluorine-containing PU performed polymer material stirrer 7, performed polymer raw material mixed solvent preheater 8, resin solvent preheater 9 resin monomer raw material premixer 10.
For ensureing that micro-nano particle can fully contact with surface-modifying agent, the stirring velocity of the particle modified high speed dispersor of micro-nano 1 is the highest can reach 3000r/min.For realizing continuous prodution, faster production, expanding the scale of production, micro-nano improving particle surface process uses the pattern of six still parallel connections, fluorine-containing Hydroxylated acrylic resin production process adopts six still series models, and fluorine-containing PU performed polymer solidifying agent production process adopts two still series model.Micro-nano improving particle surface six still reaction unit in parallel (2) is the device that reactor parallel connection that six volumes are identical uses, and six reactors successively interval 50min go into operation.Fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4 is devices that reactor pipeline that six volumes are identical is connected in sequence, and material flows in whole device.
The annexation of complete assembly is:
Described device comprises super two thin coating composition A production system and super two thin coating composition B production system; Described super two thin coating composition A production system comprises the first subsystem and the second subsystem;
Described first subsystem comprises modified particle high speed dispersor 1, modified particle six still reaction unit 2 in parallel and wet cyclone 3; Described second subsystem comprises resin monomer raw material premixer 10, fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4 and resin solvent preheater 9; Described super two thin coating composition B production system comprises fluorine-containing PU performed polymer solidifying agent two still cascade reaction device 6, performed polymer material stirrer 7 and performed polymer feed preheater 8;
Described first subsystem and the second subsystem are linked together by resin Composition A agitator 5;
In first subsystem, described modified particle high speed dispersor 1 is connected by pipeline and modified particle six still reaction unit 2 in parallel through pump, and described modified particle six still reaction unit 2 in parallel is connected with wet cyclone 3 by pipeline through pump; Described wet cyclone 3 liquid exit is connected to storage tank before the charging of modified particle high speed dispersor by pipeline, solid outlet is connected to resin Composition A agitator 5 by pipeline; Before the charging of described modified particle high speed dispersor, storage tank is connected with modified particle high speed dispersor 1 by pipeline;
In second subsystem, described resin monomer raw material premixer 10 is connected with fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4 by pipeline, described resin solvent preheater 9 is connected with fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4 by pipeline, and described fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4 is connected with resin Composition A agitator 5 by pipeline through pump;
In super two thin coating composition B production system, described performed polymer feed preheater 8 is connected with performed polymer material stirrer 7 by pipeline, and performed polymer material stirrer 7 is connected by the two still cascade reaction device 6 of pipeline and fluorine-containing PU performed polymer solidifying agent through pump.
Described modified particle six still reaction unit 2 in parallel adopts six still parallel forms, greatly can improve the throughput of subsystem 1, facilitate the maintenance of reactor simultaneously.
Described fluorine-containing Hydroxylated acrylic resin reaction unit 4 adopts multi-floating bodies reaction formation, and wherein the number of reactor is 4-8, and can make up in traditional coating production technique to rely on increases reaction kettle body sum quantity to improve the shortcoming of turnout.
Produce the Production Flow Chart of super two thin coating that 50,000 modified particles are modified per year: the utility model production process is made up of three parts, micro-nano improving particle surface production process respectively, fluorine-containing Hydroxylated acrylic resin production process and fluorine-containing PU performed polymer solidifying agent production process.
Micro-nano improving particle surface production process: enter into modified particle high speed dispersor (1) from storage tank as the ethanol (7937.5kg/h) of solvent and acetone (30.21kg/h); Raw material ten diheptyl propyl trimethoxy silicane (1143.75kg/h) enters the particle modified high speed dispersor 1 of micro-nano from head tank simultaneously; (combination of above ethanol, acetone and ten diheptyl propyl trimethoxy silicanes is the reaction liquid mixed solution marked in Fig. 3); Add vinegar acid for adjusting pH large most 4.0.
Above composition is uniformly mixed fully, enters into preheater through mixing material pump, enters into modified particle six still reaction unit 2 in parallel, add micron particle Al simultaneously after preheating
2o
3with nanoparticle SiO
2, and then make ten diheptyl propyl trimethoxy silicanes and micro-nano particle generation linked reaction (176.40kg/h).
Above-mentioned micro-nano improving particle surface reaction process reflux continues 6 hours.Arrive wet cyclone 3 by pump after mixed solution (9621.18kg/h) after reflux is first cooled by condenser, the nanoparticle of surface modification is transferred to dryer from lower port, dewaters at 120 DEG C; Get back in reactive system after reaction solution processes after testing.Finally obtain dry and carried out surface-treated nanoparticle (1320.14kg/h), being stored in storage tank for subsequent use.
Fluorine-containing Hydroxylated acrylic resin production process: before starting the reaction should under empty still state, first open nitrogen siphunculus, drive air in still away, solvent butyl acetate (958.3kg/h) and methyl iso-butyl ketone (MIBK) (275kg/h) are mixed into mixed solvent and enter storage tank, and the partial solvent accounting for mixed solvent total amount 70% is put in the reactor I of fluorine-containing Hydroxylated acrylic resin six still cascade reaction device 4 after resin solvent preheater 9 is preheating to 95 DEG C.
Raw material methyl methacrylate (MMA) (298.61kg/h), butyl acrylate (BA) (197.92kg/h), hydroxyethyl methylacrylate (HEMA) (187.5kg/h), N-BUTYL ACETATE (287.5kg/h) and initiator benzoyl peroxide (BPO) (39.58kg/h) enter into resin monomer raw material premixer 10 from head tank respectively, add mixed solvent total mass (1233.3kg/h) remaining 30% to resin monomer raw material premixer 10 simultaneously; (above methyl methacrylate (MMA), butyl acrylate (BA), hydroxyethyl methylacrylate (HEMA), N-BUTYL ACETATE and initiator benzoyl peroxide (BPO) and mixed solvent total mass remaining 30% combine the monomer mixed solution be in Fig. 3); Be transported in header tank after preliminary mixing and temporarily store; Put in reactor I 11 by monomer configurator by 70% of the mixture (1098.6kg/h) in header tank, holding temperature is 90 DEG C, and the reaction times is 50min, and still connects water trap simultaneously, removes wherein moisture by condensing reflux.
Reactor I 11 material flows into reactor II 12; Drop into reactor II 12 and drop into 10% of mixture total mass in header tank by monomer configurator, 50% of methacrylic acid ten trifluoro monooctyl ester (being the fluorine monomer in Fig. 3) (319.44kg/h) total mass is added drop-wise in reactor II 12 by configurator.Reactor II 12 reaction times is also 50min, and temperature is 90 DEG C; Still connects water trap simultaneously, removes wherein moisture by condensing reflux.
Reactor II 12 material flows into reactor III 13, and dropped into 10% of mixture total mass in header tank by monomer configurator to reactor III 13,25% of methacrylic acid ten trifluoro monooctyl ester total mass is added drop-wise in reactor III 13.The reaction times of reactor III 13 is 50min, and temperature is 90 DEG C; Still connects water trap simultaneously, removes wherein moisture by condensing reflux.
Reactor III 13 material flows into reactor IV 14.Be added drop-wise in reactor IV 14 by mixture and 25% fluorine monomer in remaining 10% header tank, the reaction times is 50min, and temperature is 90 DEG C; Still connects water trap simultaneously, removes wherein moisture by condensing reflux.
Reactor IV 14 material flows into reactor V 15, temperature of reaction is upgraded to 110 DEG C, adds thinner (acetone: N-BUTYL ACETATE mass ratio=1:4.8) (68.42kg/h) in reactor V 15, insulation 50min, still connects water trap simultaneously, removes wherein moisture by condensing reflux.In penultimate and last still, be added with film auxiliary agent and defoamer, thus be conducive to the quality-guarantee of fluorine-containing Hydroxylated acrylic resin.
Reactor V 15 material flows into reactor VI 16, add the polyether-modified type silicone antifoam agent (68.98kg/h) of SD-505 film coalescence aid (54.34kg/h), TEGOGlideB1484 flow agent (57.77kg/h) and BYC-710, insulation 50min, fluorine-containing Hydroxylated acrylic resin.Extracted out from reactor VI by fluorine-containing Hydroxylated acrylic resin through fluorine-containing Hydroxylated acrylic resin pump, transfer in monomer separation device, reflux dewatering removal of impurities removing fails to participate in the monomer reacted.Purer for gained fluorine-containing Hydroxylated acrylic resin is transferred to resin Composition A agitator 5, for next operating unit by fluorine-containing Hydroxylated acrylic resin pump.
The fluorine-containing Hydroxylated acrylic resin (having added dispersion agent, film auxiliary agent and defoamer) production upstream obtained continues to add modification micro-nano particle by proportioning (resin quality: modification micro-nano particle mass ratio=1.8:1) by configurator in resin Composition A agitator 5, high-speed stirring 30min, high speed dispersion 30min, high-speed stirring 30min again, obtains component A(2758.94kg/h); Operation is still carried out in a nitrogen environment.
Fluorine-containing PU performed polymer solidifying agent production process: solvent butyl acetate (321.88kg/h) and hexone (188.89kg/h) join mixing agitator from head tank, stir, being arrived after performed polymer raw material mixed solvent preheater 8 is heated to 70 DEG C of temperature by mixing solutions pump joins in fluorine-containing PU performed polymer material stirrer 7, and solid perfluoroalkyl ethanol (275kg/h) (being " perfluoroethanol " that mark in Fig. 3) also joins in this agitator simultaneously; After solids all dissolve, utilize flasher to remove moisture, obtain mixed solution 1.
The two still cascade reaction device 6 of fluorine-containing PU performed polymer solidifying agent should under empty still state before starting the reaction, first open nitrogen siphunculus, drive air in still away, first add mixed solution 1, header tank again by being equipped with configurator adds the mixing solutions of dibutyl tin dilaurate (catalyzer) (17.09kg/h) and HDI tripolymer (772.92kg/h) and N-BUTYL ACETATE (536.46kg/h), i.e. mixed solution 2.
Because reaction is thermopositive reaction, for avoiding reaction too fast, mixed solution 2 should slowly add, and by configurator adjust flux, mixed solution 2 points 5 batches is added in 2h.Reaction insulation 2.5h, by still temperature between the temperature control system control reaction period between 86 DEG C, then stops heating after continuing to stir 30min, allows solution be cooled to room temperature.
Because isocyanate group activity in HDI tripolymer is comparatively strong, be easy to and active hydrogen reaction in the hydroxyl in perfluoroalkyl ethanol and generate prepolymer.Completing of end reaction judges that reaction is reached home by measuring free-NCO groups content≤8% in still, from reactor discharging product component B.
Measure free-NCO groups content and adopt Di-n-Butyl Amine method.Sample about 3 grams in Erlenmeyer flask, add 15ml toluene solution and 5ml Di-n-Butyl Amine solution, leave standstill 15min, add 50ml ethanol with transfer pipet, with the hydrochloric acid-ethanolic soln titration of 0.5mol/L.-NCO group content can be obtained by the amount of the titrating solution consumed.
Claims (3)
1. a device for the super two thin coating of production of modified particle modification, is characterized in that, described device comprises super two thin coating composition A production system and super two thin coating composition B production system; Described super two thin coating composition A production system comprises the first subsystem and the second subsystem;
Described first subsystem comprises modified particle high speed dispersor (1), modified particle six still reaction unit (2) in parallel and wet cyclone (3); Described second subsystem comprises resin monomer raw material premixer (10), fluorine-containing Hydroxylated acrylic resin six still cascade reaction device (4) and resin solvent preheater (9); Described super two thin coating composition B production system comprises fluorine-containing PU performed polymer solidifying agent two still cascade reaction device (6), performed polymer material stirrer (7) and performed polymer feed preheater (8);
Described first subsystem and the second subsystem are linked together by resin Composition A agitator (5);
In first subsystem, described modified particle high speed dispersor (1) is connected by pipeline and modified particle six still reaction unit (2) in parallel through pump, and described modified particle six still reaction unit (2) in parallel is connected with wet cyclone (3) by pipeline through pump; Described wet cyclone (3) liquid exit is connected to storage tank before the charging of modified particle high speed dispersor by pipeline, solid outlet is connected to resin Composition A agitator (5) by pipeline; Before the charging of described modified particle high speed dispersor, storage tank is connected with modified particle high speed dispersor (1) by pipeline;
In second subsystem, described resin monomer raw material premixer (10) is connected with fluorine-containing Hydroxylated acrylic resin six still cascade reaction device (4) by pipeline, described resin solvent preheater (9) is connected with fluorine-containing Hydroxylated acrylic resin six still cascade reaction device (4) by pipeline, and described fluorine-containing Hydroxylated acrylic resin six still cascade reaction device (4) is connected with resin Composition A agitator (5) by pipeline through pump;
In super two thin coating composition B production system, described performed polymer feed preheater (8) is connected with performed polymer material stirrer (7) by pipeline, and performed polymer material stirrer (7) is connected by the two still cascade reaction device (6) of pipeline and fluorine-containing PU performed polymer solidifying agent through pump.
2. the device of the super two thin coating of production of modified particle modification according to claim 1, is characterized in that, described modified particle six still reaction unit (2) in parallel adopts six still parallel forms.
3. the device of the super two thin coating of production of modified particle modification according to claim 1, is characterized in that, described fluorine-containing Hydroxylated acrylic resin reaction unit (4) adopts multi-floating bodies reaction formation, and wherein the number of reactor is 4-8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315871A (en) * | 2015-11-25 | 2016-02-10 | 华南理工大学 | Device and method for producing super-amphiphobic paint with modification of modified particles |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315871A (en) * | 2015-11-25 | 2016-02-10 | 华南理工大学 | Device and method for producing super-amphiphobic paint with modification of modified particles |
| CN105315871B (en) * | 2015-11-25 | 2017-04-19 | 华南理工大学 | Device and method for producing super-amphiphobic paint with modification of modified particles |
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