CN108018543A - A kind of without phosphorus no zinc prefilming agent of recirculated cooling water and preparation method thereof - Google Patents
A kind of without phosphorus no zinc prefilming agent of recirculated cooling water and preparation method thereof Download PDFInfo
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- CN108018543A CN108018543A CN201711071833.7A CN201711071833A CN108018543A CN 108018543 A CN108018543 A CN 108018543A CN 201711071833 A CN201711071833 A CN 201711071833A CN 108018543 A CN108018543 A CN 108018543A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
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Abstract
The invention discloses without phosphorus no zinc prefilming agent of a kind of recirculated cooling water and preparation method thereof, which is made of according to mass fraction meter following component：10~30 parts of dispersant, 10~30 parts of research of non-phosphorus scale inhibitor, 1~15 part of the concentrated sulfuric acid, 40~60 parts of water.Dispersant is made of according to mass fraction meter following component：60~130 parts of cis-butenedioic anhydride, 50~90 parts of 2 acrylamide, 2 methyl propane sulfonic acid, 90~100 parts of acrylic acid, 80~150 parts of initiator, 1~10 part of molybdate, 10~30 parts of polyalcohol, 480~920 parts of water.The prefilming agent of the present invention is suitable for recirculating cooling water system, the pre- film of the cleaning of air conditioner condensation system, and cleaning speed is fast, cleaning performance is good, film forming speed is fast, form a film dense uniform, rate of corrosion are low.
Description
Technical field
It is pre- in particular to a kind of without phosphorus no zinc of recirculated cooling water the present invention relates to recirculated cooling water pre-filming treatment technical field
Film and preparation method thereof.
Background technology
The intensification of reinforcement and the contradiction of supply and demand for the water resource recently as environmentally friendly dynamics, rational utilization of water resources have become
It is particularly significant.In entire society's water, industrial water occupies very big ratio, therefore is to reasonable utilize of industrial water
Save the key point of water resource.
Pre- film is one of essential important step in Treatment of Industrial Water technique center, is to improve circulating cooling wetting system pipe
The important method of material corrosion resistance.Prefilming agent in equipment metal surface, or can changed before circulation drives operation
The metal surface for being in the state of activation after cleaning especially after pickling is learned, previously generates one layer of complete fine and close corrosion-resistant protection
Film, this is the important means for improving circulation corrosion resistance.
At present, the prefilming agent of industrial circulating cooling water processing is usually using traditional prefilming agent, i.e. Phos zinc prefilming agent, bag
Include calgon and white vitriol (15:, and sodium tripolyphosphate and white vitriol (3 4):1), dosage is higher than 300mg/
L, pre- film condition controls pH, and preliminary filming time is 36~48h between 6.5~7.2, and traditional prefilming agent use condition is harsh, pre- film
During using substantial amounts of inorganic acid for adjusting pH, it is high to water quality requirement, and discharge the high zinc of water high phosphorus and be unfavorable for environmental protection, waste water
Processing cost is higher.Therefore find a kind of not harsh to water quality requirement, be widely used and be solution to the prefilming agent of environment non-hazardous
The effective way of certainly traditional prefilming agent drawback.
Authorization Notice No. be the Chinese invention patent of CN1202028C disclose it is a kind of be used for recirculated cooling water prefilming agent and
Prefilming method, the prefilming agent are by phosphoric acid, zinc dihydrogen phosphate, containing carboxylic acid-based copolymer, organic phospho acid, benzotriazole and water group
It is when making the moisturizing of recirculating cooling water system with surface water or underground water under natural service condition (high alkalinity) into, its advantage,
Can directly pre- film, it is not necessary to acid adding or special acid adding equipment, it is not harsh to water quality requirement, but make during the prefilming agent use
Caused environment pollution with having a considerable amount of phosphorus and zinc.
The content of the invention
Present invention aim to provide without phosphorus no zinc prefilming agent of a kind of recirculated cooling water and preparation method thereof, the pre- film
Agent is without phosphorus no zinc formula, and cleaning speed is fast, cleaning performance is good, film forming speed is fast, film forming dense uniform, rate of corrosion is low, can be with
Overcome difficult water quality bad adaptability existing for existing pre- film water treatment technology, wastewater treatment, use condition harshness and high phosphorus high
The shortcomings that zinc is to environmental hazard.
To achieve the above object, the present invention provides a kind of without phosphorus no zinc prefilming agent of recirculated cooling water, it is according to mass parts
Number meter is made of following component：10~30 parts of dispersant, 10~30 parts of research of non-phosphorus scale inhibitor, 1~15 part of the concentrated sulfuric acid, water 40~60
Part,；The dispersant is prepared by the following raw material：Cis-butenedioic anhydride, 2- acrylamide-2-methyl propane sulfonics, acrylic acid, initiator,
Molybdate, polyalcohol, water.
Preferably, the without phosphorus no zinc prefilming agent of the recirculated cooling water, it is made of according to mass fraction meter following component：Point
15~25 parts of powder, 15~25 parts of research of non-phosphorus scale inhibitor, 8~12 parts of the concentrated sulfuric acid, 45~50 parts of water；The dispersant is by the following raw material
It is prepared：Cis-butenedioic anhydride, 2- acrylamide-2-methyl propane sulfonics, acrylic acid, initiator, molybdate, polyalcohol, water.
Most preferably, the without phosphorus no zinc prefilming agent of the recirculated cooling water, it is made of according to mass fraction meter following component：Point
22 parts of powder, 23 parts of research of non-phosphorus scale inhibitor, 10 parts of the concentrated sulfuric acid, 45 parts of water；The dispersant is according to mass fraction meter by the following raw material
It is prepared：Cis-butenedioic anhydride, 2- acrylamide-2-methyl propane sulfonics, acrylic acid, initiator, molybdate, polyalcohol, water.
Further, the dispersant is made of according to mass fraction meter following component：60~130 parts of cis-butenedioic anhydride, 2- propylene
It is 50~90 parts of acid amides -2- methyl propane sulfonic acids, 90~100 parts of acrylic acid, 80~150 parts of initiator, 1~10 part of molybdate, polynary
10~30 parts of alcohol, 480~920 parts of water.
Preferably, the dispersant is made of according to mass fraction meter following component：80~110 parts of cis-butenedioic anhydride, 2- acryloyls
60~80 parts of amine -2- methyl propane sulfonic acids, 92~98 parts of acrylic acid, 110~120 parts of initiator, 6~8 parts of molybdate, polyalcohol 12
~27 parts, 620~920 parts of water.
Most preferably, the dispersant is made of according to mass fraction meter following component：120 parts of cis-butenedioic anhydride, 2- acrylamides -2-
70 parts of methyl propane sulfonic acid, 96 parts of acrylic acid, 120 parts of initiator, 9 parts of molybdate, 27 parts of polyalcohol, 480~920 parts of water.
Further, one or more of the initiator in ammonium persulfate, potassium peroxydisulfate, hydrogen peroxide.
Preferably, the initiator by ammonium sulfate, potassium peroxydisulfate according to mass ratio 1:2 mix.
Preferably, the initiator by, potassium peroxydisulfate, hydrogen peroxide be according to mass ratio 1:2 mix.
Most preferably, the initiator by ammonium sulfate, potassium peroxydisulfate, hydrogen peroxide according to mass ratio 1:1:1 mixes.
Further, one or more of the molybdate in ammonium molybdate, sodium molybdate, magnesium molybdate.
Preferably, the molybdate by sodium molybdate, magnesium molybdate according to mass ratio 1:2 mix.
Preferably, the molybdate by ammonium molybdate, sodium molybdate according to mass ratio 1:2 mix.
Most preferably, the molybdate by ammonium molybdate, sodium molybdate, magnesium molybdate according to mass ratio 1:1:1 mixes.
Further, one or more of the polyalcohol in ethylene glycol, isopropanol, diethylene glycol.
Preferably, the polyalcohol by isopropanol, diethylene glycol according to mass ratio 1:2 mix.
Preferably, the polyalcohol by ethylene glycol, isopropanol according to mass ratio 1:2 mix
Most preferably, the polyalcohol by ethylene glycol, isopropanol, diethylene glycol according to mass ratio 1:1:1 mixes.
Further, the molecular weight ranges of the dispersant are 2000~4000.
Further, the synthetic route of the dispersant is as follows：
Wherein：M is Na2MOO4, x is the integer in 2~10, and y is the integer in 2~10, and z is the integer in 2~10.
Further, the preparation method of the dispersant includes the following steps：Added according to the mass fraction into reactor
60~130 parts of cis-butenedioic anhydrides and 100~400 parts of water, are warming up to 60~100 DEG C after mixing, then into reactor be added dropwise 50~
90 parts of 2- acrylamide-2-methyl propane sulfonics, 90~100 parts of acrylic acid and 300~400 parts of water mixed solutions, and be slowly added dropwise
80~150 parts of initiators and 1~10 part of molybdate, keep the temperature 1~3h at 80~90 DEG C after being added dropwise, are cooled to after insulation
Room temperature adds 10~30 parts of polyalcohols, 80~120 parts of water after mixing, obtains dispersant.
Further, the research of non-phosphorus scale inhibitor is polyepoxy sodium succinate and/or poly-aspartate.
Preferably, the research of non-phosphorus scale inhibitor by polyepoxy sodium succinate and poly-aspartate according to mass ratio 1：1 mixing and
Into.
Further, the mass concentration of the concentrated sulfuric acid is 90~98.3%.
Present invention also offers a kind of preparation method of the above-mentioned without phosphorus no zinc prefilming agent of recirculated cooling water, including following step
Suddenly：
Weigh according to the mass fraction 10~30 parts of dispersants, 10~30 parts of research of non-phosphorus scale inhibitor, 1~15 part of concentrated sulfuric acid, 40~
60 parts of water are uniformly mixed, and acid solution is added dropwise and adjusts appearance untill transparent clear, you can.
Further, the acid solution is selected from one or both of hydrochloric acid, sulfuric acid；Wherein, the quality of the hydrochloric acid
Concentration is 25~37%；The mass concentration of the sulfuric acid is 37~40%.
Compared with prior art, prefilming agent of the invention carries out dispersion mixing by the degradable dispersant of biology, has
The characteristics of environmentally protective without phosphorus no zinc, will not cause natural water eutrophic harm, polymerized monomer used biology easily drop
Solution.The dispersant used in prefilming agent is that cis-butenedioic anhydride and water are mixed into solution A；By 2- acrylamide-2-methyl propane sulfonics, propylene
Acid is mixed into solution B with water；Then solution B is slowly added dropwise in solution A, while a small amount of initiator is added dropwise, and keep temperature
Degree reacts 1~3h, synthetic intermediate C at 60~100 DEG C；Finally intermediate is mixed with a small amount of polynary alcohol and water at normal temperatures
To final dispersant.Obtained dispersant and research of non-phosphorus scale inhibitor and a small amount of concentrated sulfuric acid are compounded, using the result shows that：This is pre-
Film has the advantage that：(1) it is suitable for recirculating cooling water system, the pre- film of the cleaning of air conditioner condensation system, it is not severe to water quality requirement
Carve, be widely used；(2) cleaning speed is fast, cleaning performance is good, film forming speed is fast, form a film dense uniform, rate of corrosion are low；(3) it is without phosphorus
Without zinc formula, environmentally protective safety.
Embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
10 parts, 20 parts of research of non-phosphorus scale inhibitor (PESA polyepoxy sodium succinates), 6.5 parts of the concentrated sulfuric acid (mass concentration 98.3%), 60 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：60 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
50 parts of sulfonic acid, 90 parts of acrylic acid, 140 parts of initiator (ammonium sulfate), 8 parts of molybdate (ammonium molybdate), 10 parts of polyalcohol (isopropanol),
580 parts of water.
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
60 parts of cis-butenedioic anhydrides and 160 parts of water are added according to the mass fraction into reactor, are warming up to 85 DEG C after mixing, then
50 parts of 2- acrylamide-2-methyl propane sulfonics, 90 parts of acrylic acid and 300 parts of water mixed solutions are added dropwise into reactor, and slowly
140 parts of initiators and 8 parts of molybdates are added dropwise, 1.5h is kept the temperature at 85 DEG C after being added dropwise, controls rate of addition and reaction temperature, makes
The molecular weight for obtaining product is cooled to room temperature 10 parts of isopropanols of addition after 2000, insulation, and 120 parts of water obtain after mixing
Dispersant；
(2) compounding of prefilming agent：
Weigh according to the mass fraction by 10 parts of dispersants, 20 parts of PESA polyepoxy sodium succinates, 6.5 parts of concentrated sulfuric acids, 60 parts
Water is uniformly mixed, and adjusts appearance untill transparent clear with hydrochloric acid solution (mass concentration 25%), you can.
Embodiment 2：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
20 parts, 25 parts of research of non-phosphorus scale inhibitor (PASP poly-aspartates), 5 parts of the concentrated sulfuric acid (mass concentration 98.3%), 50 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：45 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
67 parts of sulfonic acid, 95 parts of acrylic acid, 90 parts of initiator (ammonium sulfate), 6 parts of molybdate (ammonium molybdate), 12 parts of polyalcohol (isopropanol),
570 parts of water.
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 45 parts of cis-butenedioic anhydrides and 150 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, Ran Houxiang
67 parts of 2- acrylamide-2-methyl propane sulfonics, 95 parts of acrylic acid and 300 parts of water mixed solutions are added dropwise in reactor, and slowly drip
Add 90 parts of initiators and 6 parts of molybdate solutions, 2.0h kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature,
So that the molecular weight of product be cooled to after 2200, insulation room temperature add 12 parts of isopropanols, 120 parts of water after mixing,
Obtain dispersant；
(2) compounding of prefilming agent：
20 parts of dispersants, 25 parts of PASP poly-aspartates, 5 parts of concentrated sulfuric acids, 50 parts of water mixing are weighed according to the mass fraction
It is even, and appearance is adjusted untill transparent clear with sulfuric acid (mass concentration 40%) solution, you can.
Embodiment 3：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
22 parts, 23 parts of research of non-phosphorus scale inhibitor, 10 parts of the concentrated sulfuric acid (mass concentration 98.3%), 45 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：120 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
(initiator is by ammonium sulfate, potassium peroxydisulfate, hydrogen peroxide according to mass ratio 1 for 70 parts of sulfonic acid, 96 parts of acrylic acid, initiator:1:1 mixing
Into) 120 parts, (molybdate is by ammonium molybdate, sodium molybdate, magnesium molybdate according to mass ratio 1 for molybdate:1:1 mixes) 9 parts, it is more
(polyalcohol is by ethylene glycol, isopropanol, diethylene glycol according to mass ratio 1 for first alcohol:1:1 mixes) 27 parts, 920 parts of water；
Research of non-phosphorus scale inhibitor is by polyepoxy sodium succinate and poly-aspartate according to mass ratio 1：1 mixes；
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 130 parts of cis-butenedioic anhydrides and 400 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, then
90 parts of 2- acrylamide-2-methyl propane sulfonics, 100 parts of acrylic acid and 400 parts of water mixed solutions are added dropwise into reactor, and slowly
150 parts of initiators and 10 parts of molybdate solutions are added dropwise, 2.0h is kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature
Degree so that the molecular weight of product is cooled to 30 parts of polyalcohols of room temperature addition after 4000, insulation, 120 parts of water are uniformly mixed
Afterwards, dispersant is obtained；
(2) compounding of prefilming agent：
30 parts of dispersants, 20 parts of research of non-phosphorus scale inhibitor, 10 parts of concentrated sulfuric acids, 40 parts of water are weighed according to the mass fraction to be uniformly mixed,
And appearance is adjusted untill transparent clear with sulfuric acid solution (mass concentration 37%), you can.
Embodiment 4：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
10 parts, 30 parts of research of non-phosphorus scale inhibitor, 15 parts of the concentrated sulfuric acid (mass concentration 98.3%), 45 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：60 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
(initiator is by ammonium sulfate, potassium peroxydisulfate according to mass ratio 1 for 50 parts of sulfonic acid, 90 parts of acrylic acid, initiator:2 mix) 80 parts,
(molybdate is by ammonium molybdate, sodium molybdate according to mass ratio 1 for molybdate:2 mix) 1 part, polyalcohol (polyalcohol by ethylene glycol,
Isopropanol is according to mass ratio 1:2 mix) 10 parts, 480 parts of water；
Research of non-phosphorus scale inhibitor is by polyepoxy sodium succinate and poly-aspartate according to mass ratio 1：1 mixes；
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 60 parts of cis-butenedioic anhydrides and 100 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, Ran Houxiang
50 parts of 2- acrylamide-2-methyl propane sulfonics, 90 parts of acrylic acid and 300 parts of water mixed solutions are added dropwise in reactor, and slowly drip
Add 80 parts of initiators and 1 part of molybdate solution, 2.0h kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature,
So that the molecular weight of product is cooled to room temperature after 2000, insulation and adds 10 parts of polyalcohols, 80 parts of water after mixing, obtain
To dispersant；
(2) compounding of prefilming agent：
10 parts of dispersants, 30 parts of research of non-phosphorus scale inhibitor, 15 parts of concentrated sulfuric acids, 45 parts of water are weighed according to the mass fraction to be uniformly mixed,
And with hydrochloric acid solution (mass concentration 37%) and sulfuric acid solution (mass concentration 37%) according to 1:The acid solution tune of 1 mixing
Appearance is saved untill transparent clear, you can.
Embodiment 5：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
15 parts, 25 parts of research of non-phosphorus scale inhibitor, 10 parts of the concentrated sulfuric acid (mass concentration 98.3%), 50 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：80 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
60 parts of sulfonic acid, 92 parts of acrylic acid, initiator (initiator by, potassium peroxydisulfate, hydrogen peroxide be according to mass ratio 1:2 mix) 110
Part, (molybdate is by sodium molybdate, magnesium molybdate according to mass ratio 1 for molybdate:2 mix) 6 parts, (polyalcohol is by isopropyl for polyalcohol
Alcohol, diethylene glycol are according to mass ratio 1:2 mix) 12 parts, 780 parts of water；
Research of non-phosphorus scale inhibitor is by polyepoxy sodium succinate and poly-aspartate according to mass ratio 1：1 mixes；
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 80 parts of cis-butenedioic anhydrides and 300 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, Ran Houxiang
60 parts of 2- acrylamide-2-methyl propane sulfonics, 92 parts of acrylic acid and 400 parts of water mixed solutions are added dropwise in reactor, and slowly drip
Add 110 parts of initiators and 6 parts of molybdate solutions, 2.0h kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature,
So that the molecular weight of product is cooled to room temperature after 3000, insulation and adds 12 parts of polyalcohols, 80 parts of water after mixing, obtain
To dispersant；
(2) compounding of prefilming agent：
15 parts of dispersants, 25 parts of research of non-phosphorus scale inhibitor, 10 parts of concentrated sulfuric acids, 50 parts of water are weighed according to the mass fraction to be uniformly mixed,
And appearance is adjusted untill transparent clear with sulfuric acid solution (mass concentration 37%), you can.
Embodiment 6：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
25 parts, 15 parts of research of non-phosphorus scale inhibitor, 12 parts of the concentrated sulfuric acid (mass concentration 98.3%), 48 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：110 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
(initiator is by ammonium sulfate, hydrogen peroxide according to mass ratio 1 for 80 parts of sulfonic acid, 98 parts of acrylic acid, initiator:2 mix) 120 parts,
(molybdate is by ammonium molybdate, magnesium molybdate according to mass ratio 1 for molybdate:2 mix) 8 parts, polyalcohol (polyalcohol by ethylene glycol,
Diethylene glycol is according to mass ratio 1:2 mix) 25 parts, 620 parts of water；
Research of non-phosphorus scale inhibitor is by polyepoxy sodium succinate and poly-aspartate according to mass ratio 1：1 mixes；
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 110 parts of cis-butenedioic anhydrides and 200 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, then
98 parts of 2- acrylamide-2-methyl propane sulfonics, 98 parts of acrylic acid and 300 parts of water mixed solutions are added dropwise into reactor, and slowly
120 parts of initiators and 8 parts of molybdate solutions are added dropwise, 2.0h is kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature
Degree so that the molecular weight of product is cooled to 25 parts of polyalcohols of room temperature addition after 4000, insulation, 120 parts of water are uniformly mixed
Afterwards, dispersant is obtained；
(2) compounding of prefilming agent：
25 parts of dispersants, 15 parts of research of non-phosphorus scale inhibitor, 12 parts of concentrated sulfuric acids, 48 parts of water are weighed according to the mass fraction to be uniformly mixed,
And appearance is adjusted untill transparent clear with sulfuric acid solution (mass concentration 37%), you can.
Embodiment 7：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
25 parts, 15 parts of research of non-phosphorus scale inhibitor (poly-aspartate), 12 parts of the concentrated sulfuric acid (mass concentration 90%), 48 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：110 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
80 parts of sulfonic acid, 98 parts of acrylic acid, 120 parts of initiator (hydrogen peroxide), 8 parts of molybdate (magnesium molybdate), polyalcohol (diethylene glycol) 25
Part, 620 parts of water.
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 110 parts of cis-butenedioic anhydrides and 200 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, then
98 parts of 2- acrylamide-2-methyl propane sulfonics, 98 parts of acrylic acid and 300 parts of water mixed solutions are added dropwise into reactor, and slowly
120 parts of initiators and 8 parts of molybdate solutions are added dropwise, 2.0h is kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature
Degree so that the molecular weight of product is cooled to 25 parts of polyalcohols of room temperature addition after 4000, insulation, 120 parts of water are uniformly mixed
Afterwards, dispersant is obtained；
(2) compounding of prefilming agent：
25 parts of dispersants, 15 parts of research of non-phosphorus scale inhibitor, 12 parts of concentrated sulfuric acids, 48 parts of water are weighed according to the mass fraction to be uniformly mixed,
And appearance is adjusted untill transparent clear with sulfuric acid solution (mass concentration 37%), you can.
Embodiment 8：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
30 parts, 20 parts of research of non-phosphorus scale inhibitor (polyepoxy sodium succinate), 10 parts of the concentrated sulfuric acid (mass concentration 98.3%), 40 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：130 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
90 parts of sulfonic acid, 100 parts of acrylic acid, 150 parts of initiator (potassium peroxydisulfate), 10 parts of molybdate (sodium molybdate), polyalcohol (ethylene glycol)
30 parts, 920 parts of water.
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 130 parts of cis-butenedioic anhydrides and 400 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, then
90 parts of 2- acrylamide-2-methyl propane sulfonics, 100 parts of acrylic acid and 400 parts of water mixed solutions are added dropwise into reactor, and slowly
150 parts of initiators and 10 parts of molybdate solutions are added dropwise, 2.0h is kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature
Degree so that the molecular weight of product is cooled to 30 parts of polyalcohols of room temperature addition after 4000, insulation, 120 parts of water are uniformly mixed
Afterwards, dispersant is obtained；
(2) compounding of prefilming agent：
30 parts of dispersants, 20 parts of research of non-phosphorus scale inhibitor, 10 parts of concentrated sulfuric acids, 40 parts of water are weighed according to the mass fraction to be uniformly mixed,
And appearance is adjusted untill transparent clear with sulfuric acid solution (mass concentration 37%), you can.
Embodiment 9：
The without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water, is made of according to mass fraction meter following component：Dispersant
27 parts, 23 parts of research of non-phosphorus scale inhibitor (poly-aspartate), 2 parts of the concentrated sulfuric acid (mass concentration 90%), 48 parts of water.
Wherein, dispersant is made of according to mass fraction meter following component：110 parts of cis-butenedioic anhydride, 2- acrylamide -2- methyl-props
80 parts of sulfonic acid, 98 parts of acrylic acid, 120 parts of initiator (hydrogen peroxide), 8 parts of molybdate (magnesium molybdate), polyalcohol (diethylene glycol) 25
Part, 620 parts of water.
The preparation method of the without phosphorus no zinc prefilming agent of the present embodiment recirculated cooling water：
(1) preparation of dispersant：
Add 110 parts of cis-butenedioic anhydrides and 200 parts of water in the reactor by mass fraction, be warming up to 85 DEG C after mixing, then
98 parts of 2- acrylamide-2-methyl propane sulfonics, 98 parts of acrylic acid and 300 parts of water mixed solutions are added dropwise into reactor, and slowly
120 parts of initiators and 8 parts of molybdate solutions are added dropwise, 2.0h is kept the temperature at 85 DEG C after being added dropwise, control rate of addition and reaction temperature
Degree so that the molecular weight of product is cooled to 25 parts of polyalcohols of room temperature addition after 4000, insulation, 120 parts of water are uniformly mixed
Afterwards, dispersant is obtained；
(2) compounding of prefilming agent：
27 parts of dispersants, 23 parts of research of non-phosphorus scale inhibitor, 2 parts of concentrated sulfuric acids, 48 parts of water are weighed according to the mass fraction to be uniformly mixed, and
Appearance is adjusted untill transparent clear with hydrochloric acid solution (mass concentration 37%), you can.
1~9 prepared prefilming agent of above-described embodiment is directly added into experimental water and carries out rotary hanging plate experiment, is added dense
300mg/L, 45 DEG C, test period 48h of test temperature are spent, test water water quality is：Ca2+(with CaCO3Meter) 147mg/L, total alkali
Degree is (with CaCO3Meter) 104.2mg/L, Cl-75mg/L, SO4 2-35.2mg/L, pH7.62, experimental result are shown in Table 1.
Comparative example：By the drug concentration of calgon 200mg/L, zinc sulfate 100mg/L be added in experimental water into
Row rotary hanging plate is tested, 45 DEG C, test period 48h of test temperature, during experiment with sulfuric acid control experimental water pH value 5.5~
Between 6.5.Test water water quality is：Ca2+(with CaCO3Meter) 147mg/L, total alkalinity is (with CaCO3Meter) 104.2mg/L, Cl-
75mg/L, SO4 2-35.2mg/L, pH7.62, experimental result are shown in Table 1.
1 prefilming agent effect test result of table
Product dependence test：
1st, materialization is tested：Carbon steel coupon, stainless steel substrates and the copper sheet after the pre- film of prefilming agent can be observed using electron microscope
On have densification protective film, carbon steel is most thick, secondly be copper sheet.
2nd, electro-chemical test：Pre- film belongs to absorbent-type protective film made of the prefilming agent.
The above description is merely a specific embodiment, it is noted that any those skilled in the art exist
Disclosed herein technical scope in, the change or replacement that can readily occur in, should all cover protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of without phosphorus no zinc prefilming agent of recirculated cooling water, it is characterised in that it is made of according to mass fraction meter following component：
10~30 parts of dispersant, 10~30 parts of research of non-phosphorus scale inhibitor, 1~15 part of the concentrated sulfuric acid, 40~60 parts of water；The dispersant is by following former
Material is prepared：Cis-butenedioic anhydride, 2- acrylamide-2-methyl propane sulfonics, acrylic acid, initiator, molybdate, polyalcohol, water.
2. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 1, it is characterised in that the dispersant is according to matter
Amount number meter is prepared by the following raw material：60~130 parts of cis-butenedioic anhydride, 50~90 parts of 2- acrylamide-2-methyl propane sulfonics, propylene
90~100 parts of acid, 80~150 parts of initiator, 1~10 part of molybdate, 10~30 parts of polyalcohol, 480~920 parts of water.
3. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 2, it is characterised in that the initiator was selected from
One or more in ammonium sulfate, potassium peroxydisulfate, hydrogen peroxide.
4. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 2, it is characterised in that the molybdate is selected from molybdenum
One or more in sour ammonium, sodium molybdate, magnesium molybdate.
5. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 2, it is characterised in that the polyalcohol is selected from second
One or more in glycol, isopropanol, diethylene glycol.
6. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 2, it is characterised in that the synthesis of the dispersant
Route is as follows：
Wherein：M is Na2MOO4, x is the integer in 2~10, and y is the integer in 2~10, and z is the integer in 2~10.
7. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 2, it is characterised in that the preparation of the dispersant
Method includes the following steps：60~130 parts of cis-butenedioic anhydrides and 100~400 parts of water are added according to the mass fraction into reactor, mixing is equal
60~100 DEG C are warming up to after even, 50~90 parts of 2- acrylamide-2-methyl propane sulfonics, 90~100 are then added dropwise into reactor
Part acrylic acid and 300~400 parts of water mixed solutions, and 80~150 parts of initiators and 1~10 part of molybdate is slowly added dropwise, it is added dropwise
After 80~90 DEG C keep the temperature 1~3h, be cooled to after insulation room temperature add 10~30 parts of polyalcohols, 80~120 parts of water
After mixing, dispersant is obtained.
8. the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 1, it is characterised in that the research of non-phosphorus scale inhibitor is
Polyepoxy sodium succinate and/or poly-aspartate.
9. the preparation method of the without phosphorus no zinc prefilming agent of recirculated cooling water described in a kind of claim 1, it is characterised in that including as follows
Step：Weigh according to the mass fraction 10~30 parts of dispersants, 10~30 parts of research of non-phosphorus scale inhibitor, 1~15 part of concentrated sulfuric acid, 40~60 parts
Water is uniformly mixed, and acid solution is added dropwise and adjusts appearance untill transparent clear, you can.
10. the preparation method of the without phosphorus no zinc prefilming agent of recirculated cooling water according to claim 9, it is characterised in that the acid
Property solution be selected from hydrochloric acid solution, one or both of sulfuric acid solution；Wherein, the mass concentration of the hydrochloric acid solution for 25~
37%；The mass concentration of the sulfuric acid solution is 37~40%.
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| CN113699516A (en) * | 2021-08-27 | 2021-11-26 | 洛阳强龙实业有限公司 | Circulating cooling water phosphorus-free prefilming agent and application thereof |
| CN114086167A (en) * | 2021-11-11 | 2022-02-25 | 新疆水处理工程技术研究中心有限公司 | Non-phosphorus prefilming agent and preparation method thereof |
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