CN110003393A - A kind of water-repellent preservation macromolecule emulsion and its production technology - Google Patents
A kind of water-repellent preservation macromolecule emulsion and its production technology Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/06—Propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/04—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene copolymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/06—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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Abstract
The invention belongs to the preparation technical fields of macromolecule emulsion, it is related to a kind of water-repellent preservation macromolecule emulsion and its production technology, the production technology of the lotion are as follows: weigh solvent, major catalyst and co-catalyst and be placed in reaction kettle, be mixed evenly, be configured to organic solution；It weighs monomer to be added in organic solution, stirs 4~16h, synthesize atactic polyolefin；Random copolymer is heated to 140~280 DEG C, adjusts 0.4~4MPa of pressure, initiator, grafted monomers are added under agitation, benzimidazole and tert-butyl hydroperoxide is then added, continues to be stirred to react 2-4h；After reaction, solvent is removed, soap lye is added and is stirred, is then 9-10 with the pH value of ammonium hydroxide adjustment mixed material, obtains the water-repellent preservation macromolecule emulsion.Water-repellent preservation macromolecule emulsion of the invention has good caking property, is not easy to peel off, and with excellent thermal stability and certain antibacterial, antimicrobial corrosivity.
Description
Technical field
The invention belongs to the preparation technical field of macromolecule emulsion, it is related to a kind of water-repellent preservation macromolecule emulsion and its production
Technique.
Background technique
Corrosion protection is safety problem, is economic problems, is the major issue of national economy.The famous marine corrosion in China and protection
Researcher, Chinese Academy of Engineering Hou Baorong academician point out that China's corrosion cost in 2014 is about in " China's corrosion cost " book
2.1 trillion RMB, account for about the 3.34% of current year GDP, and the corrosion cost that every citizen mutually should bear current year is
1555 yuan, this is a very surprising number.Corrosion protection is in aerospace, sea transport, the fields such as infrastructure to pass
Important, to steel, profile, alloy, it is the key subjects of national defense construction and national economy that timber etc., which does necessary protective treatment,.
Cause the factor of corrosion failure very much, carbon dioxide, sulfur dioxide, microorganism, water, salt, dust in air etc.
Deng the corrosion and consumption of material can be caused.The corrosion protection of normal conventional depends on the integrality of protective film, the unfavorable pole of environment
Destructible protective film.Such as paint, completely cut off air and water, substantially prolongs by the service life of protection matrix.But protecting film is resistance to
Aging determines the effective protection phase, and the protecting film of organic matter and the coefficient of thermal expansion and contraction of metal material have very big difference,
Temperature change, by shock of external force etc., rigid protecting film is easy to destroy or even localized delamination, in addition microorganism is broken
It is bad, so as to cause protection failure.
Summary of the invention
The present invention to solve the above-mentioned problems, provides a kind of water-repellent preservation macromolecule emulsion and its production technology, the water
Property anti-corrosion macromolecule emulsion there is good caking property, be not easy to peel off, and have excellent thermal stability and certain antibacterial,
Antimicrobial corrosivity.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of production technology of water-repellent preservation macromolecule emulsion, comprising the following steps:
(1) solvent, major catalyst and co-catalyst are weighed to be placed in reaction kettle, is mixed evenly, is configured to organic molten
Liquid；
(2) it weighs monomer to be added in the organic solution in reaction kettle, stirs 4~16h, synthesize atactic polyolefin；
(3) atactic polyolefin in reaction kettle is heated to 140~280 DEG C, 0.4~4MPa of pressure is adjusted, in stirring bar
Initiator, grafted monomers are added under part, benzimidazole and tert-butyl hydroperoxide is then added, continues to be stirred to react 2-4h；
(4) after reaction, solvent is removed, soap lye is added and is stirred, then with the pH value of ammonium hydroxide adjustment mixed material
For 9-10, the water-repellent preservation macromolecule emulsion is obtained.
A kind of production technology of water-repellent preservation macromolecule emulsion as described above, the solvent are the alkanes of Long carbon chain
Or the cycloalkane of saturation, the major catalyst are to remember in Chinese invention patent that Authorization Notice No. is CN 101942053B
The catalyst of load, the co-catalyst are triethyl aluminum, and the major catalyst and co-catalyst are raw material gross weight
0.0005%, 0.0025%.
A kind of production technology of water-repellent preservation macromolecule emulsion as described above, in step (2), the monomer is second
Alkene, propylene, 1- butylene, two or more in isobutene, the mass ratio of the monomer and solvent is 1:2.
A kind of production technology of water-repellent preservation macromolecule emulsion as described above in the step (2), weighs monomer addition
In organic solution in reaction kettle, after reacting 30min, it is passed through hydrogen, is stirred to react 4~16h under the conditions of 120~240 DEG C, closed
At atactic polyolefin.
A kind of production technology of water-repellent preservation macromolecule emulsion as described above, in step (3), the initiator is
AIBN, the dosage of the initiator are the 0.02% of atactic polyolefin weight, and the grafted monomers are acrylic acid, and the grafting is single
The dosage of body is the 5% of atactic polyolefin weight, and the initiator, grafted monomers are added completely into reaction kettle in 2~4h.Its
In, the AIBN, which is dissolved in, to be configured in the AIBN solution addition reaction kettle that concentration is 10% in solvent, and acrylic acid is dissolved in solvent
The acrylic acid solution that concentration is 50% is configured to be added in reaction kettle.
A kind of production technology of water-repellent preservation macromolecule emulsion as described above, in step (3), the use of the benzimidazole
Amount is the 1% of atactic polyolefin weight, and the mass ratio of the tert-butyl hydroperoxide and benzimidazole is 1:10.Wherein, described
Benzimidazole, which is dissolved in, to be configured in the benzimidazole solution addition reaction kettle that concentration is 40% in solvent, the tert-butyl hydroperoxide
Hydrogen is dissolved in the tert-butyl hydroperoxide solution that compound concentration is 5% in dimethylbenzene and is added in reaction kettle.
A kind of production technology of water-repellent preservation macromolecule emulsion as described above, in step (4), after reaction, by object
Material is distilled under the conditions of 120 DEG C, 0.05MPa, removes solvent.
The invention also discloses the water-repellent preservation high scores that the production technology by above-mentioned water-repellent preservation macromolecule emulsion produces
Sub- lotion.The backbone structure of the water-repellent preservation macromolecule emulsion is the polyolefin of random copolymerization flexible, on the main chain
It is inlaid with methyl, ethyl, propyl, carboxyl, amino, benzimidazole functional group.
The invention also discloses above-mentioned water-repellent preservation macromolecule emulsion corrosion-resistant field application.
The alkene of water-repellent preservation macromolecule emulsion low pole of the invention synthesizes main chain, and main chain is high fluidity, amorphous
The flexible olefin copolymer of state, high degree of randomness；Certain density is inlaid with the bases such as methyl, ethyl, propyl, carboxyl, amino on main chain
Group, the soft main chain of these alkyl groups cooperation, plays the role of repulsion water, water, oxygen, microorganism, these carboxyls, amino is isolated
Group plays the role of adsorbing with metal-polar, adhere to.
But the polyolefin backbone of the random copolymerization of this softness both made generally with the bonding force of metal surface and insecure
There is the polarity of carboxyl to adsorb, bonding force is not also enough, and the present inventor makees on main chain by being grafted a certain amount of benzimidazole
To anchor functional group, so that polarity of chain is reached certain level, promote material to the bonding force of metal.Benzimidazole itself
It is a kind of antimicrobial Specific potent compounds of sterilization, aqueous solution specific anti-corrosion effects make after the present invention is by reaction
It is grafted with benzimidazole functional group on main chain, after benzimidazole functional group is grafted on main chain, still there are enough freedom degrees, plays
The effect of functional group, antimicrobial corrosion reach certain rust-proof effect.
Beneficial effects of the present invention:
Water-repellent preservation macromolecule emulsion of the invention is emulsion type, has good room temperature tack, hot melting cohesion, pressure
Quick caking property and uvioresistant, resistance to ag(e)ing can construct as spray painting, directly in humidity or can have dirty surface to spray
Covering construction is applied, protecting film anti-high and low-temp, vibration resistance, the impact of resistance to sandstone can be with long-acting lasting protection, to cement steel, steel
Rail, iron sheet, timber can all greatly prolong its service life.
Water-repellent preservation macromolecule emulsion of the invention also has outstanding high and low temperature performance and temperature-insensitive, can
It is used in -50 DEG C~+100 DEG C temperature ranges；Filmogen flexible makes coating have apparent automatic healing properties, does not have
The Minute pores of solvent based coating.
Water-repellent preservation macromolecule emulsion of the invention also has good restraining and sterilizing bacteria and antimicrobial corrosivity, application
Range is extremely wide.
Detailed description of the invention
Fig. 1 is the hcl corrosion test effect schematic diagram of water-repellent preservation macromolecule emulsion made from embodiment 1.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies specific structure, process conditions and its result described in example and is merely to illustrate the present invention without right should will not be limited
The present invention described in detail in claim.
Embodiment 1
A kind of production technology of water-repellent preservation macromolecule emulsion, comprising the following steps:
(1) normal heptane, hexahydrotoluene, major catalyst and co-catalyst are weighed to be placed in autoclave, is mixed
Uniformly, it is configured to organic solution, wherein the mass ratio of normal heptane and hexahydrotoluene is 1:1, and the major catalyst is for making
(Authorization Notice No. is embodiment in the Chinese invention patent of CN101942053B to the effective catalyst of standby high random olefin copolymers
The catalyst of 1 preparation), the co-catalyst is triethyl aluminum, and the dosage of the major catalyst and co-catalyst is raw material gross weight
0.0005%, the 0.0025% of amount；
(2) ethylene, propylene, 1- butylene, isobutene are weighed to be passed through in autoclave, is passed through hydrogen after being stirred to react 30min
Gas continues to be stirred to react under the conditions of 120 DEG C 8h, synthesize atactic polyolefin, wherein ethylene, propylene, 1- butylene, isobutene
The mass ratio of total dosage and solvent is 1:2, ethylene, propylene, 1- butylene, isobutene mass percent be 25%:65%:5%:
5%；
(3) AIBN and heptane are weighed, the AIBN n-heptane solution that AIBN concentration is 10% is configured to；Weigh acrylic acid and heptan
Alkane is configured to the acrylic acid n-heptane solution that acrylic acid concentration is 50%；Benzimidazole and heptane are weighed, it is dense to be configured to benzimidazole
The benzimidazole n-heptane solution that degree is 40%；Weigh tert-butyl hydroperoxide and dimethylbenzene, the tert-butyl mistake that compound concentration is 5%
Hydrogen peroxide solution；Weigh appropriate potassium hydroxide, OP-10 is dissolved in hot water, preparation obtain 90 DEG C of soap lye, it is spare, wherein
The dosage of AIBN is the 0.02% of atactic polyolefin weight, and the dosage of acrylic acid is the 5% of atactic polyolefin weight, benzimidazole
Dosage be the 1% of atactic polyolefin weight, the mass ratio of tert-butyl hydroperoxide and benzimidazole is 1:10；
(4) atactic polyolefin in autoclave is heated to 140 DEG C, adjusting pressure is 0.5MPa, in stirring condition
The lower AIBN n-heptane solution and acrylic acid n-heptane solution for being slowly pumped into step (3) preparation simultaneously into autoclave, control pump
Enter speed so that AIBN n-heptane solution and acrylic acid n-heptane solution have been pumped into 4h, is then pumped into step (3) preparation simultaneously again
Benzimidazole n-heptane solution and tert-butyl hydroperoxide solution, be stirred to react 4h；
(5) after reaction, mixed material is distilled under the conditions of 120 DEG C, 0.05MPa, removes solvent, then will
The material for removing solvent is placed in reaction kettle, and soap lye emulsion reaction 2h step (3) prepared is added under the conditions of 90 DEG C, then uses
The pH value that ammonium hydroxide adjusts mixed material is 9, controls the solid content of material between 40%~60%, obtains the water-repellent preservation
Macromolecule emulsion.
A kind of production technology water-repellent preservation macromolecule emulsion produced of water-repellent preservation macromolecule emulsion described above.
A kind of application of water-repellent preservation macromolecule emulsion described above in corrosion-resistant field.
Embodiment 2
A kind of production technology of water-repellent preservation macromolecule emulsion, comprising the following steps:
(1) octane, major catalyst and co-catalyst are weighed to be placed in autoclave, is mixed evenly, has been configured to
Machine solution, wherein the major catalyst is to be used to prepare the effective catalysts of high random olefin copolymers (Authorization Notice No. is
The catalyst that in the Chinese invention patent of CN101942053B prepared by embodiment 1), the co-catalyst is triethyl aluminum, described
The dosage of major catalyst and co-catalyst is 0.0005%, the 0.0025% of raw material gross weight；
(2) ethylene, propylene, isobutene are weighed to be passed through in autoclave, hydrogen is passed through after being stirred to react 30min, 180
Continue to be stirred to react 4h under the conditions of DEG C, synthesizes atactic polyolefin, wherein ethylene, propylene, total dosage of isobutene and the matter of solvent
Amount than be 1:2, ethylene, propylene, isobutene mass percent be 30%:65%:5%；
(3) AIBN and octane are weighed, the AIBN octane solution that AIBN concentration is 10% is configured to；Weigh acrylic acid and pungent
Alkane is configured to the acrylic acid octane solution that acrylic acid concentration is 50%；Benzimidazole and octane are weighed, it is dense to be configured to benzimidazole
The benzimidazole octane solution that degree is 40%；Weigh tert-butyl hydroperoxide and dimethylbenzene, the tert-butyl mistake that compound concentration is 5%
Hydrogen peroxide solution；Weigh appropriate potassium hydroxide, OP-10 is dissolved in hot water, preparation obtain 70 DEG C of soap lye, it is spare, wherein
The dosage of AIBN is the 0.02% of atactic polyolefin weight, and the dosage of acrylic acid is the 5% of atactic polyolefin weight, benzimidazole
Dosage be the 1% of atactic polyolefin weight, the mass ratio of tert-butyl hydroperoxide and benzimidazole is 1:10；
(4) atactic polyolefin in autoclave is heated to 200 DEG C, adjusting pressure is 2MPa, under agitation
It is slowly pumped into the AIBN octane solution of step (3) preparation simultaneously into autoclave and acrylic acid octane solution, control are pumped into
Then speed is pumped into step (3) preparation so that AIBN octane solution and acrylic acid octane solution have been pumped into 4h simultaneously again
Benzimidazole octane solution and tert-butyl hydroperoxide solution, are stirred to react 2h；
(5) after reaction, mixed material is distilled under the conditions of 120 DEG C, 0.05MPa, removes solvent, then will
The material for removing solvent is placed in reaction kettle, and soap lye emulsion reaction 2h step (3) prepared is added under the conditions of 90 DEG C, then uses
The pH value that ammonium hydroxide adjusts mixed material is 10, controls the solid content of material between 40%~60%, is obtained described aqueous anti-
Rotten macromolecule emulsion.
A kind of production technology water-repellent preservation macromolecule emulsion produced of water-repellent preservation macromolecule emulsion described above.
A kind of application of water-repellent preservation macromolecule emulsion described above in corrosion-resistant field.
Embodiment 3
A kind of production technology of water-repellent preservation macromolecule emulsion, comprising the following steps:
(1) hexane, methyl cyclopentane, major catalyst and co-catalyst are weighed to be placed in autoclave, is mixed equal
It is even, be configured to organic solution, wherein the hexane, methyl cyclopentane mass ratio be 2:1, the major catalyst be for making
(Authorization Notice No. is embodiment in the Chinese invention patent of CN101942053B to the effective catalyst of standby high random olefin copolymers
The catalyst of 1 preparation), the co-catalyst is triethyl aluminum, and the dosage of the major catalyst and co-catalyst is raw material gross weight
0.0005%, the 0.0025% of amount；
(2) ethylene, propylene, 1- butylene are weighed to be passed through in autoclave, hydrogen is passed through after being stirred to react 30min, 240
Continue to be stirred to react 4h under the conditions of DEG C, synthesize atactic polyolefin, wherein ethylene, propylene, the gross mass of 1- butylene and solvent matter
Amount than be 1:2, ethylene, propylene, 1- butylene mass percent be 25%:70%:5%；
(3) AIBN and hexane are weighed, the AIBN hexane solution that AIBN concentration is 10% is configured to；Weigh acrylic acid and oneself
Alkane is configured to the acrylic acid hexane solution that acrylic acid concentration is 50%；Benzimidazole and hexane are weighed, it is dense to be configured to benzimidazole
The benzimidazole hexane solution that degree is 40%；Weigh tert-butyl hydroperoxide and dimethylbenzene, the tert-butyl mistake that compound concentration is 5%
Hydrogen peroxide solution；Weigh appropriate potassium hydroxide, OP-10 is dissolved in hot water, preparation obtain 95 DEG C of soap lye, it is spare, wherein
The dosage of AIBN is the 0.02% of atactic polyolefin weight, and the dosage of acrylic acid is the 5% of atactic polyolefin weight, benzimidazole
Dosage be the 1% of atactic polyolefin weight, the mass ratio of tert-butyl hydroperoxide and benzimidazole is 1:10；
(4) atactic polyolefin in autoclave is heated to 280 DEG C, adjusting pressure is 4MPa, under agitation
It is slowly pumped into the AIBN octane solution of step (3) preparation simultaneously into autoclave and acrylic acid octane solution, control are pumped into
Then speed is pumped into step (3) preparation so that AIBN hexane solution and acrylic acid hexane solution have been pumped into 2h simultaneously again
Benzimidazole hexane solution and tert-butyl hydroperoxide solution, are stirred to react 3h；
(5) after reaction, mixed material is distilled under the conditions of 120 DEG C, 0.05MPa, removes solvent, then will
The material for removing solvent is placed in reaction kettle, and soap lye emulsion reaction 2h step (3) prepared is added under the conditions of 90 DEG C, then uses
The pH value that ammonium hydroxide adjusts mixed material is 9, controls the solid content of material between 40%~60%, obtains the water-repellent preservation
Macromolecule emulsion.
A kind of production technology water-repellent preservation macromolecule emulsion produced of water-repellent preservation macromolecule emulsion described above.
A kind of application of water-repellent preservation macromolecule emulsion described above in corrosion-resistant field.
Performance test:
One, neutral salt spray test
Salt spray test inspection is carried out to water-repellent preservation macromolecule emulsion of the invention according to ASTM-B117 salt spray test standard
It surveys, after testing, the coating of water-repellent preservation macromolecule emulsion brushing of the invention is continuously exposed to concentration under the conditions of 35 DEG C and is
In 5% salt fog, after continuous exposure in 500 hours, coating appearance is good, without fall off, aliquation, hollowing, cracking phenomena.
Two, hcl corrosion is tested
The metal plate of two pieces of onesize same materials is taken, is made in one of metal plate spraying embodiment of the present invention 1
Water-repellent preservation macromolecule emulsion, as experimental group, another piece of metal plate is without any processing, as blank control group.Normal
Under temperature, the metal plate of experimental group and blank control group is soaked in the hydrochloric acid solution that concentration is 5% respectively, is taken after impregnating three days
Out, the etch state of the metal plate of experimental group and control group is as shown in Figure 1, wherein the left side metal plate in Fig. 1 is experimental group spray
The metal plate of water-repellent preservation macromolecule emulsion obtained in embodiment 1 is applied, the metal plate on right side is that blank control group is not done and sprayed
Painting processing, after the metal plate of experimental group impregnates three days in 5% hydrochloric acid solution, good-looking, nothing fall off, aliquation, hollowing,
Cracking phenomena, and the metal plate of blank control group has the falling off of large area, hollowing phenomenon, has the area greater than 30% to be corroded,
Prove that water-repellent preservation macromolecule emulsion of the invention has good acid-proof anticorrosive effect.
Three, antibacterial tests
Experimental strain: Candida albicans Candida albicans (ATCC 10231)
Preparation bacterium solution: saving in strain test tube from 3 platinite candida albicans and take an oese, draws on sabouraud's agar plate
Line for 24 hours in 37 ± 1 DEG C of cultures chooses colonies typical with oese from plate, it is oblique to be inoculated in sabouraud's agar test tube
Face for 24 hours in 37 ± 1 DEG C of cultures, then 5mL 0.03mol/L PBS buffer solution is added into test tube, and pressure-vaccum, washes down fresh bacterium repeatedly
Then eluent is moved in desinfection chamber pipe with suction pipe, is mixed well by tongue fur, viable count 1 × 10 is made8The inoculation bacterium of CFU/mL is outstanding
Liquid.
The appropriate examination for moving into and 0.03mol/L PBS buffer solution being housed is drawn from Candida albicans inoculation bacteria suspension with suction pipe
Guan Zhong is diluted to viable count 2.5 × 105~3 × 105The Candida albicans of CFU/mL is inoculated with bacterium solution.
Prepare 12 250mL conical flasks, every three are one group, are added in every group in wherein three groups of conical flasks white
Color candida albicans is inoculated with water-repellent preservation macromolecule emulsion made from bacterium solution 5mL, 0.03mol/L PBS buffer solution 70mL, embodiment 1-3
Candida albicans inoculation bacterium solution 5mL, 0.03mol/L PBS is respectively added as test group, in the other three conical flask by 0.75g
Buffer 70mL covers bottle stopper as blank control group, and conical flask is placed on constant temperature oscillator, at 24 DEG C, 150r/min
Vibrate 18h.1mL bacterium solution is taken from each flask, is moved into the test tube equipped with 9mL 0.03mol/L PBS buffer solution, it is sufficiently mixed
It is even.It is serially diluted with 10 times of dilution methods to suitable multiple, then draws 0.2mL and cultivate 48h in sabouraud's agar, do three
A Duplicate Samples measure viable count by the method for GB/T 4789.2.After being oscillation 18h multiplied by extension rate by the viable count of measurement
Actual recovered viable bacteria numerical value.
Calculate bacteriostasis rate:
Bacteriostasis rate presses formula: Y=(W-Q)/W × 100% is calculated,
In formula:
Y-sample bacteriostasis rate；
W-blank control group is averaged bacterial count recovered；
Q-experimental group is averaged bacterial count recovered.
The results are shown in Table 1 for antibacterial tests.
1 antibacterial tests data of table
From data it is found that water anti-bacteria coating of the invention has good the bacteriostasis rate > 90% of Candida albicans
Inhibit antifungal effect.
The technical concepts and features of embodiment of above only to illustrate the invention, its object is to allow be familiar with technique
People understands the content of present invention and is implemented, and it is not intended to limit the scope of the present invention, and all spirit according to the present invention is real
The equivalent change or modification that matter is done should all be contained in lid protection scope of the present invention.
Claims (9)
1. a kind of production technology of water-repellent preservation macromolecule emulsion, which comprises the following steps:
(1) solvent, major catalyst and co-catalyst are weighed to be placed in reaction kettle, is mixed evenly, is configured to organic solution；
(2) it weighs monomer to be added in the organic solution in reaction kettle, stirs 4~16h, synthesize atactic polyolefin；
(3) atactic polyolefin in reaction kettle is heated to 140~280 DEG C, adjusts 0.4~4MPa of pressure, under agitation
Initiator, grafted monomers is added, benzimidazole and tert-butyl hydroperoxide is then added, continues to be stirred to react 2-4h；
(4) after reaction, solvent is removed, soap lye is added and is stirred, is then 9- with the pH value of ammonium hydroxide adjustment mixed material
10, obtain the water-repellent preservation macromolecule emulsion.
2. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1, which is characterized in that described is molten
Agent is the alkanes of Long carbon chain or the cycloalkane of saturation, and the major catalyst is that Authorization Notice No. is 101942053 B of CN
Chinese invention patent in the catalyst recorded, the co-catalyst is triethyl aluminum, the major catalyst and co-catalyst
Dosage be raw material gross weight 0.0005%, 0.0025%.
3. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1, which is characterized in that step (2)
In, the monomer is ethylene, propylene, 1- butylene, two or more in isobutene, and the mass ratio of the monomer and solvent is
1:2。
4. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1, which is characterized in that the step
(2) it in, weighs monomer and is added in the organic solution in reaction kettle, after reacting 30min, hydrogen is passed through, in 120~240 DEG C of conditions
Under be stirred to react 4~16h, synthesize atactic polyolefin.
5. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1, which is characterized in that step (3)
In, the initiator is AIBN, and the dosage of the initiator is the 0.02% of atactic polyolefin weight, and the grafted monomers are third
Olefin(e) acid, the dosage of the grafted monomers are the 5% of atactic polyolefin weight, and the initiator, grafted monomers are added in 2~4h
In reaction kettle.
6. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1, which is characterized in that step (3)
In, the dosage of the benzimidazole is the 1% of atactic polyolefin weight, the quality of the tert-butyl hydroperoxide and benzimidazole
Than for 1:10.
7. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1, which is characterized in that step (4)
In, after reaction, material is distilled under the conditions of 120 DEG C, 0.05MPa, removes solvent.
8. a kind of production technology of water-repellent preservation macromolecule emulsion according to claim 1-7 produces aqueous anti-
Rotten macromolecule emulsion.
9. a kind of water-repellent preservation macromolecule emulsion according to any one of claims 8 is in the application of corrosion-resistant field.
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| CN110862485A (en) * | 2019-11-19 | 2020-03-06 | 合众（佛山）化工有限公司 | APAO modified waterborne acrylic resin and preparation method thereof |
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