CN103319645A - Water-based metallic protective agent and productive technology thereof - Google Patents

Water-based metallic protective agent and productive technology thereof Download PDF

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Publication number
CN103319645A
CN103319645A CN2013102125276A CN201310212527A CN103319645A CN 103319645 A CN103319645 A CN 103319645A CN 2013102125276 A CN2013102125276 A CN 2013102125276A CN 201310212527 A CN201310212527 A CN 201310212527A CN 103319645 A CN103319645 A CN 103319645A
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reactor
monomer
massfraction
add
added
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CN2013102125276A
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CN103319645B (en
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骆光达
张钊
王金文
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NANJING JIEYA NEW MATERIAL Co Ltd
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NANJING JIEYA NEW MATERIAL Co Ltd
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Abstract

The invention provides a water-based metallic protective agent. The water-based metallic protective agent comprises monomers, molecular weight adjusting agents and initiators. The monomers comprise methyl methacrylate with a mass fraction of 20%-40%, butyl acrylate with a mass fraction of 20%-40%, acrylic acid with a mass fraction of 10%-18%, phenylethylene with a mass fraction of 5%-15%, and hydroxyethyl acrylate with a mass fraction of 8%-15%. The additive mass of the molecular weight adjusting agents is 0.1%-2% of the total mass of the monomers. The additive mass of the initiators is 0.1%-5% of the total mass of the monomers. The invention further provides a productive technology of the water-based metallic protective agent. The water-based metallic protective agent and the productive technology thereof take water as a solvent. The water-based metallic protective agent does not contain any organic solvents or heavy metal ions, replaces heavy-metal-ion and solvent-cotaining metal surface treatment agents in the prior art and reduces pollution.

Description

A kind of part aqueous metal protection agent and production technique thereof
Technical field
The present invention relates to the aqueous product technical field, particularly a kind of part aqueous metal protection agent and production technique thereof.
Background technology
Present domestic part aqueous metal protection agent produce market is mainly dominated by Japan, German company.And the rate of utilization of the aqueous product of main American-European countries is more than 70%, and domestic rate of utilization is less than 30%, and market potential is huge.Under the international big environment of the environmental consciousness that constantly strengthens, in following 5-10, the use aqueous product can be with the speed increment of annual 5%-8%.There are the problems such as seriously polluted in the metal conditioner that contains at present heavy metal ion and solvent based.
Summary of the invention
The present invention proposes a kind of part aqueous metal protection agent and production technique thereof, take water as solvent, does not contain any organic solvent and heavy metal ion, and alternative present stage contains the metal conditioner of heavy metal ion and solvent based, reduces and pollutes.The technical solution adopted in the present invention specifically is achieved in that
The invention provides a kind of part aqueous metal protection agent; it comprises monomer, molecular weight adjusting agent and initiator; described monomer comprises that massfraction is that the methyl methacrylate of 20%-40%, the butyl acrylate that massfraction is 20%-40%, the vinylformic acid that massfraction is 10%-18%, vinylbenzene and the massfraction that massfraction is 5%-15% are the Hydroxyethyl acrylate of 8%-15%; the amount that described molecular weight adjusting agent is added is the 0.1%-2% of described monomer total mass, and the amount that described initiator adds is the 0.1%-5% of described monomer total mass.
In the specific embodiment of the invention, the amount that described molecular weight adjusting agent is added is the 0.1%-2% of described monomer total mass, and the amount that described initiator adds is the 0.1%-5% of described monomer total mass.
On the other hand, the invention provides a kind of production technique of part aqueous metal protection agent, it comprises step:
A. check production unit and other facilities;
B. monomer and molecular weight adjusting agent are mixed and stir stand-byly, described monomer comprises that massfraction is that 35% methyl methacrylate, massfraction are that 35% butyl acrylate, massfraction are that 12% vinylformic acid, massfraction are that 8% vinylbenzene and massfraction are 10% Hydroxyethyl acrylate;
C. a certain amount of active carrier is added in the reactor, stir and be heated to design temperature;
D. take out a certain amount of in the mix monomer from step b and proportionally add initiator, add in the reactor after the stirring and dissolving, be warming up to 85 ℃-90 ℃, when solution occuring refluxing, insulation reaction 30-40 minute, open simultaneously cooling;
E. initiator and stirring and dissolving will proportionally be added in the remaining monomer among the process b, in the gob barrel of packing into;
F. after the steps d reaction, with Temperature Setting at 100 ℃, and after being warming up to 100 ℃-103 ℃, open the tear drop valve, begin to drip mix monomer in reactor, control monomer dropping speed, be added dropwise to complete in 3 hours, insulation reaction 30 minutes proportionally adds active carrier and initiator, insulation reaction 3 hours;
G. stir after reactor temperature being cooled to 45 ℃-50 ℃, and proportionally add neutralizing agent, time for adding 40 minutes insulation reaction 40-60 minute, is got product and is detected and be: water-soluble clarification, pH value 7.0-8.0;
H. a certain proportion of deionized water is added in the reactor, and add a certain proportion of BTA, churning time 30-40 minute;
I. product in the reactor is emitted, and look different customer requirements, add deionized water or other auxiliary agents of different ratios, stir;
J. pack.
In the specific embodiment of the invention, comprise the inspection that reactor stopping property, stirring system, heating temperature-control system, water cooling system, feed back are received and drip the material system among the described step a.
In the specific embodiment of the invention, among the described step c, the 170Kg active carrier is added in the reactor, opens and stir and heating temperature-control system, and Temperature Setting at 85 ℃.
In the specific embodiment of the invention, in the described steps d, from mix monomer, take out 100Kg, add initiator 1.4Kg, and add in the reactor after the stirring and dissolving, be warming up to 85 ℃-90 ℃, when the solution backflow occurs, insulation reaction 30-40 minute, open simultaneously cooling.
In the specific embodiment of the invention, among the described step e, will add the 2.8Kg initiator in the remaining monomer among the step b, stirring and dissolving is in the gob barrel of packing into.
In the specific embodiment of the invention, among the described step f, Temperature Setting at 100 ℃, and after being warming up to 100 ℃-103 ℃, is opened the tear drop valve, begin to drip mix monomer in reactor, control monomer dropping speed was added dropwise to complete insulation reaction 30 minutes in 3 hours, add 170Kg active carrier and 1.4Kg initiator, insulation reaction 3 hours.
In the specific embodiment of the invention, in the described step g, stir after reactor temperature is cooled to 45 ℃-50 ℃, add the 20-50Kg neutralizing agent, time for adding 40 minutes insulation reaction 40-60 minute, is got product and is detected and be: water-soluble clarification, pH value 7.0-8.0.
In the specific embodiment of the invention, among the described step h, the 400Kg deionized water is added in the reactor, and added the 10-12KgBTA churning time 30-40 minute; In the described step I, product in the reactor is emitted, and look different customer requirements, add deionized water 100-500Kg or other auxiliary agents, stir.
Part aqueous metal protection agent of the present invention and production technique thereof take water as solvent, do not contain any organic solvent and heavy metal ion, and alternative present stage contains the metal conditioner of heavy metal ion and solvent based, reduce and pollute.
Embodiment
The invention provides a kind of part aqueous metal protection agent; it comprises monomer, molecular weight adjusting agent and initiator; monomer comprises that massfraction is that the methyl methacrylate of 20%-40%, the butyl acrylate that massfraction is 20%-40%, the vinylformic acid that massfraction is 10%-18%, vinylbenzene and the massfraction that massfraction is 5%-15% are the Hydroxyethyl acrylate of 8%-15%; the amount that the molecular weight adjusting agent is added is the 0.1%-2% of monomer total mass, and the amount that initiator adds is the 0.1%-5% of described monomer total mass.
In the specific embodiment of the invention, the amount that the molecular weight adjusting agent is added is the 0.1%-2% of monomer total mass, and the amount that initiator adds is the 0.1%-5% of described monomer total mass.
On the other hand, the invention provides a kind of production technique of part aqueous metal protection agent, it comprises step:
A. check production unit and other facilities;
B. monomer and molecular weight adjusting agent are mixed and stir stand-byly, described monomer comprises that massfraction is that 35% methyl methacrylate, massfraction are that 35% butyl acrylate, massfraction are that 12% vinylformic acid, massfraction are that 8% vinylbenzene and massfraction are 10% Hydroxyethyl acrylate;
C. a certain amount of active carrier is added in the reactor, stir and be heated to design temperature;
D. take out a certain amount of in the mix monomer from step b and proportionally add initiator, add in the reactor after the stirring and dissolving, be warming up to 85 ℃-90 ℃, when solution occuring refluxing, insulation reaction 30-40 minute, open simultaneously cooling;
E. initiator and stirring and dissolving will proportionally be added in the remaining monomer among the process b, in the gob barrel of packing into;
F. after the steps d reaction, with Temperature Setting at 100 ℃, and after being warming up to 100 ℃-103 ℃, open the tear drop valve, begin to drip mix monomer in reactor, control monomer dropping speed, be added dropwise to complete in 3 hours, insulation reaction 30 minutes proportionally adds active carrier and initiator, insulation reaction 3 hours;
G. stir after reactor temperature being cooled to 45 ℃-50 ℃, and proportionally add neutralizing agent, time for adding 40 minutes insulation reaction 40-60 minute, is got product and is detected and be: water-soluble clarification, pH value 7.0-8.0;
H. a certain proportion of deionized water is added in the reactor, and add a certain proportion of BTA, churning time 30-40 minute;
I. product in the reactor is emitted, and look different customer requirements, add deionized water or other auxiliary agents of different ratios, stir;
J. pack.
In the specific embodiment of the invention, the monomer total amount is 300Kg, and concrete proportioning is as shown in table 1 below:
Sequence number The monomer title Chemical name Massfraction % Weight Kg
1 Methyl methacrylate MMA 35 105
2 Butyl acrylate BA 35 105
3 Vinylformic acid AA 12 36
4 Vinylbenzene St 8 24
5 Hydroxyethyl acrylate HEA 10 30
6 The molecular weight adjusting agent AMSB 1 3
7 Initiator BOP 1.86 4.8
In the specific embodiment of the invention, the active carrier total amount of employing is 340Kg, and concrete reaction process and order of addition(of ingredients) control are as follows:
Comprise the inspection that reactor stopping property, stirring system, heating temperature-control system, water cooling system, feed back are received and drip the material system among the step a.
Among the step c, the 170Kg active carrier is added in the reactor, opens and stir and heating temperature-control system, and Temperature Setting at 85 ℃.
In the steps d, from mix monomer, take out 100Kg, add initiator 1.4Kg, and add in the reactor after the stirring and dissolving, be warming up to 85 ℃-90 ℃, when the solution backflow occurs, insulation reaction 30-40 minute, open simultaneously cooling.
Among the step e, will add the 2.8Kg initiator in the remaining monomer among the step b, stirring and dissolving is in the gob barrel of packing into.
Among the step f, with Temperature Setting at 100 ℃, and after being warming up to 100 ℃-103 ℃, open the tear drop valve, begin to drip mix monomer in reactor, control monomer dropping speed, be added dropwise to complete in 3 hours, insulation reaction 30 minutes adds 170Kg active carrier and 1.4Kg initiator, insulation reaction 3 hours.
In the step g, stir after reactor temperature is cooled to 45 ℃-50 ℃, add 20-50Kg neutralizing agent (for example ammoniacal liquor), time for adding 40 minutes insulation reaction 40-60 minute, is got product and is detected and be: water-soluble clarification, pH value 7.0-8.0.
Among the step h, the 400Kg deionized water is added in the reactor, and added the 10-12KgBTA churning time 30-40 minute; In the described step I, product in the reactor is emitted, and look different customer requirements, add deionized water 100-500Kg or other auxiliary agents, stir.
Carry out at last packaging step i.
Part aqueous metal protection agent of the present invention and production technique thereof take water as solvent, do not contain any organic solvent and heavy metal ion, and alternative present stage contains the metal conditioner of heavy metal ion and solvent based, reduce and pollute.
The present invention is of many uses in fields such as metal protection, electrolytic coating protection, application pre-treatment; the technical indicator of these series product level that is in a leading position at home; successively by the ISO9001 international quality system authentication and smoothly by the Rohs detection, product has obtained the International Environmental Protection approval.Advantage of the present invention mainly is: take water as solvent, do not contain any organic solvent and heavy metal ion, can substitute the metal conditioner that contains heavy metal ion and solvent based fully.Do not need expensive sewage treatment facility; Integrate functional and ornamental, through the metallic surface after this product treatment, the coating etch resistant properties improves more than 2 times, surface brightness improves 1-2 grade, and color and luster is lasting.
Part aqueous metal protection agent product is mainly used in precoating operation behind the electrolytic coating; its purpose is to make it to have the functions such as resistant, anti-fingerprint, anti-corrosion, bright property, anti-discolouration, high adhesive force, and the final corrosion resistant sheet material that forms is widely used in the household electric appliances such as automobile industry, computer, refrigerator, washing machine, mobile phone.The present invention can substitute the metal conditioner that present stage contains heavy metal ion and solvent based, greatly reduces pollution.
In above description, a lot of details have been set forth so that fully understand the present invention.But above description only is preferred embodiment of the present invention, and the present invention can implement much to be different from alternate manner described here, so the present invention is not subjected to the restriction of top disclosed implementation.Any skilled personnel are not breaking away from the technical solution of the present invention scope situation simultaneously, all can utilize method and the technology contents of above-mentioned announcement that technical solution of the present invention is made many possible changes and modification, or be revised as the equivalent embodiment of equivalent variations.Every content that does not break away from technical solution of the present invention according to any simple modification, equivalent variations and the modification that technical spirit of the present invention is done above embodiment, all still belongs in the scope of technical solution of the present invention protection.

Claims (10)

1. part aqueous metal protection agent; it is characterized in that; comprise monomer, molecular weight adjusting agent and initiator; described monomer comprises that massfraction is that the methyl methacrylate of 20%-40%, the butyl acrylate that massfraction is 20%-40%, the vinylformic acid that massfraction is 10%-18%, vinylbenzene and the massfraction that massfraction is 5%-15% are the Hydroxyethyl acrylate of 8%-15%; the amount that described molecular weight adjusting agent is added is the 0.1%-2% of described monomer total mass, and the amount that described initiator adds is the 0.1%-5% of described monomer total mass.
2. part aqueous metal protection agent according to claim 1 is characterized in that, the amount that described molecular weight adjusting agent is added is the 0.1%-2% of described monomer total mass, and the amount that described initiator adds is the 0.1%-5% of described monomer total mass.
3. the production technique of a part aqueous metal protection agent is characterized in that, comprises step:
A. check production unit and other facilities;
B. monomer and molecular weight adjusting agent are mixed and stir stand-byly, described monomer comprises that massfraction is that 35% methyl methacrylate, massfraction are that 35% butyl acrylate, massfraction are that 12% vinylformic acid, massfraction are that 8% vinylbenzene and massfraction are 10% Hydroxyethyl acrylate;
C. a certain amount of active carrier is added in the reactor, stir and be heated to design temperature;
D. take out a certain amount of in the mix monomer from step b and proportionally add initiator, add in the reactor after the stirring and dissolving, be warming up to 85 ℃-90 ℃, when solution occuring refluxing, insulation reaction 30-40 minute, open simultaneously cooling;
E. initiator and stirring and dissolving will proportionally be added in the remaining monomer among the process b, in the gob barrel of packing into;
F. after the steps d reaction, with Temperature Setting at 100 ℃, and after being warming up to 100 ℃-103 ℃, open the tear drop valve, begin to drip mix monomer in reactor, control monomer dropping speed, be added dropwise to complete in 3 hours, insulation reaction 30 minutes proportionally adds active carrier and initiator, insulation reaction 3 hours;
G. stir after reactor temperature being cooled to 45 ℃-50 ℃, and proportionally add neutralizing agent, time for adding 40 minutes insulation reaction 40-60 minute, is got product and is detected and be: water-soluble clarification, pH value 7.0-8.0;
H. a certain proportion of deionized water is added in the reactor, and add a certain proportion of BTA, churning time 30-40 minute;
I. product in the reactor is emitted, and look different customer requirements, add deionized water or other auxiliary agents of different ratios, stir;
J. pack.
4. the production technique of part aqueous metal protection agent according to claim 3 is characterized in that, comprises the inspection that reactor stopping property, stirring system, heating temperature-control system, water cooling system, feed back are received and drip the material system among the described step a.
5. the production technique of part aqueous metal protection agent according to claim 3 is characterized in that, among the described step c, 170 Kg active carriers is added in the reactor, open and stir and heating temperature-control system, and Temperature Setting at 85 ℃.
6. the production technique of part aqueous metal protection agent according to claim 3; it is characterized in that; in the described steps d; from mix monomer, take out 100Kg, add initiator 1.4 Kg, and add in the reactor after the stirring and dissolving; be warming up to 85 ℃-90 ℃; when the solution backflow occurs, insulation reaction 30-40 minute, open simultaneously cooling.
7. the production technique of part aqueous metal protection agent according to claim 3 is characterized in that, among the described step e, will add 2.8 Kg initiators in the remaining monomer among the step b, and stirring and dissolving is in the gob barrel of packing into.
8. the production technique of part aqueous metal protection agent according to claim 3; it is characterized in that, among the described step f, with Temperature Setting at 100 ℃; and after being warming up to 100 ℃-103 ℃; open the tear drop valve, begin to drip mix monomer in reactor, control monomer dropping speed; be added dropwise to complete in 3 hours; insulation reaction 30 minutes adds 170Kg active carrier and 1.4Kg initiator, insulation reaction 3 hours.
9. the production technique of part aqueous metal protection agent according to claim 3; it is characterized in that; in the described step g; stir after reactor temperature is cooled to 45 ℃-50 ℃; add 20-50 Kg neutralizing agent; time for adding 40 minutes insulation reaction 40-60 minute, is got product and is detected and to be: water-soluble clarification, pH value 7.0-8.0.
10. the production technique of part aqueous metal protection agent according to claim 3 is characterized in that, among the described step h, 400 Kg deionized waters is added in the reactor, and added the 10-12KgBTA churning time 30-40 minute; In the described step I, product in the reactor is emitted, and look different customer requirements, add deionized water 100-500Kg or other auxiliary agents, stir.
CN201310212527.6A 2013-05-31 2013-05-31 A kind of part aqueous metal protection agent and production technology thereof Active CN103319645B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838271A (en) * 2003-10-14 2010-09-22 辉瑞产品公司 Two ring [3.1.0] derivatives as glycine transporter inhibitors
CN102199240A (en) * 2011-03-17 2011-09-28 北京化工大学 Preparation method of styrene-acrylate copolymer emulsion used in antirust paint
CN102993840A (en) * 2011-09-19 2013-03-27 天津科技大学 Preparation technique of environment-friendly water-based rust inhibitor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838271A (en) * 2003-10-14 2010-09-22 辉瑞产品公司 Two ring [3.1.0] derivatives as glycine transporter inhibitors
CN102199240A (en) * 2011-03-17 2011-09-28 北京化工大学 Preparation method of styrene-acrylate copolymer emulsion used in antirust paint
CN102993840A (en) * 2011-09-19 2013-03-27 天津科技大学 Preparation technique of environment-friendly water-based rust inhibitor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陶金铸等: ""金属闪光涂料用水性丙烯酸树脂的合成及性能"", 《热固性树脂》 *

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