CN108034938B - Method for phosphorizing bolt of nuclear power equipment and phosphorizing liquid - Google Patents

Method for phosphorizing bolt of nuclear power equipment and phosphorizing liquid Download PDF

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Publication number
CN108034938B
CN108034938B CN201711350842.XA CN201711350842A CN108034938B CN 108034938 B CN108034938 B CN 108034938B CN 201711350842 A CN201711350842 A CN 201711350842A CN 108034938 B CN108034938 B CN 108034938B
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bolt
washing
phosphating
nuclear power
water
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CN108034938A (en
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林继德
王宏印
张斌
高俊根
马培锋
吴义党
乔木
杨志鹏
朱从斌
陈洪
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China General Nuclear Power Corp
China Nuclear Power Engineering Co Ltd
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China General Nuclear Power Corp
China Nuclear Power Engineering Co Ltd
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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
    • C23C22/73—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 characterised by the process
    • 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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/18—Orthophosphates containing manganese cations

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  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

The invention discloses a method for phosphorizing a bolt of nuclear power equipment, which comprises the following steps: s1, preprocessing the equipment bolt: firstly, soaking a bolt in deoiling liquid for deoiling treatment, washing the bolt at normal temperature after deoiling, washing the bolt with hydrochloric acid after washing, washing the bolt with water again after washing, and then performing surface conditioning; s2, soaking the pretreated bolt in a phosphating solution for a first preset time to carry out pre-phosphating; s3, reprocessing the pre-phosphorized bolt: washing the bolt with water again, washing with hydrochloric acid after washing with water, washing with water again after washing with acid, and then performing surface conditioning; and S4, soaking the retreated bolt in the phosphating solution again for a second preset time to perform phosphating. The invention also provides a phosphating solution. The phosphorization method and the phosphorization liquid for the nuclear power equipment bolt provided by the invention can obtain the nuclear power equipment bolt phosphorization layer with reliable quality, uniformity, compactness and good corrosion resistance.

Description

Method for phosphorizing bolt of nuclear power equipment and phosphorizing liquid
Technical Field
The invention relates to a phosphating treatment process, in particular to a method for phosphating bolts of nuclear power equipment and phosphating solution
Background
In a nuclear power plant, a bolt assembly is the most important fastener of nuclear island main equipment such as a reactor pressure vessel, a steam generator and the like of a nuclear power plant. According to relevant manufacturing standards, a layer of phosphating film is required to be manufactured on the surface of the bolt, so that the friction coefficient of the bolt is improved, the bolt and the nut are prevented from being seized, and a certain antirust effect is achieved. Phosphating is a process for producing a layer of non-metallic attachments on a metal surface and is a chemical and physical change process, and the quality of a phosphate coating can be seriously affected by the out-of-control of any factor in the process.
The nuclear power product has higher requirement on the phosphate coating, the phosphate coating quality of manholes, eye holes, hand hole bolts and the like of the existing nuclear power equipment is unstable, and the problems of drop of the phosphate coating, local whitening of the phosphate coating and the like exist. The phosphating layer has many subdivisions according to the components of the phosphating film, the phosphating films used in different industries are different, the key parameters of different phosphating films are different, and meanwhile, the phosphating layer is greatly influenced by the key parameters. The bolt component adopts high-temperature manganese series phosphorization, the film is heavy, and the phosphorization difficulty is large.
Therefore, the method and the phosphating solution for phosphating the nuclear power equipment bolt are provided to obtain the nuclear power equipment bolt phosphating layer with reliable quality, and are the problems to be solved in the field of nuclear power bolt phosphating at present.
Disclosure of Invention
Aiming at the problems of high-temperature manganese series phosphating, large film and high phosphating difficulty of bolts in the prior art, the invention provides a method and a phosphating solution for phosphating bolts of nuclear power equipment, and the phosphating solution can obtain the phosphating layer of the bolts of the nuclear power equipment, which has reliable quality, uniformity, compactness and good corrosion resistance.
The invention provides a method for phosphorizing a bolt of nuclear power equipment, which comprises the following steps:
s1, preprocessing the equipment bolt: firstly, soaking a bolt in deoiling liquid for deoiling treatment, washing the bolt at normal temperature after deoiling, washing the bolt with hydrochloric acid after washing, washing the bolt with water again after washing, and then performing surface conditioning;
s2, soaking the pretreated bolt in a phosphating solution for a first preset time to carry out pre-phosphating;
s3, reprocessing the pre-phosphorized bolt: washing the bolt with water again, washing with hydrochloric acid after washing with water, washing with water again after washing with acid, and then performing surface conditioning;
and S4, soaking the retreated bolt in the phosphating solution again for a second preset time to perform phosphating.
Preferably, the method further comprises the steps of:
s5, post-processing the phosphated bolt: washing the bolt with water again, passivating the bolt with a passivating agent after washing with water, washing the bolt with water again after passivating, and drying the bolt to soak oil;
and S6, carrying out quality inspection on the phosphated bolt.
Preferably, in step S2 and step S4, the same phosphating solution is used for pre-phosphating and phosphating, and the phosphating solution comprises: the additive comprises 35g/L of Marshall salt, 20g/L of manganese nitrate and 3-5g/L of accelerator;
wherein the accelerator is selected from one or more of nitrite, nitrate or chlorate.
Preferably, the total acidity of the phosphating solution is 30-40 points, the acidity of the free acid is 3-4 points, and the temperature of the pre-phosphating in the step S2 and the temperature of the phosphating process in the step S4 are both 80-90 ℃.
Preferably, the first preset time period is 10-15 minutes.
Preferably, the second preset time period is 20-25 minutes.
Preferably, the step S1 is specifically:
soaking the bolt in deoiling liquid for deoiling treatment, wherein the deoiling liquid has the temperature of 80-90 ℃ and the deoiling time of 25-30 minutes, and the deoiling liquid comprises the following components: NaOH with a concentration of 30g/l, Na3PO4 with a concentration of 30g/l and Na2CO3 with a concentration of 40 g/l;
washing the deoiled bolt with water at normal temperature;
pickling the washed bolt with 15% HCl at normal temperature for 12-20 min;
washing the bolt after acid washing again at normal temperature;
and (4) performing surface adjustment on the bolt subjected to water cleaning again by adopting a surface adjusting liquid, wherein the PH control target of the surface adjusting liquid is 8, and the surface adjusting time is 1 minute.
Preferably, the step S3 is specifically:
washing the bolt with water at normal temperature;
pickling the washed bolt with 15% HCl at normal temperature for 12-20 min;
and (4) performing surface adjustment on the bolt subjected to water cleaning again by adopting a surface adjusting liquid, wherein the PH control target of the surface adjusting liquid is 8, and the surface adjusting time is 1 minute.
Preferably, the step S5 is specifically:
washing the bolt with water at normal temperature;
after washing, passivating by using a passivating agent with the concentration of 40g/L2Cr2O7The solution is passivated for 2 minutes at 60-70 ℃.
After passivation, washing the bolt with water again;
the bolts were dried and immersed in engine oil for 4 minutes at 110-.
The invention also provides a phosphating solution for pre-phosphating and phosphating bolts of nuclear power equipment, which comprises the following components in percentage by weight: the additive comprises 35g/L of Marshall salt, 20g/L of manganese nitrate and 3-5g/L of accelerator;
wherein the accelerator is selected from one or more of nitrite, nitrate or chlorate.
Preferably, the total acidity of the phosphating solution is between 30 and 40 points.
Preferably, the acidity of the free acid of the phosphating solution is 3-4 points.
One or more technical schemes provided by the scheme of the invention at least have the following technical effects or advantages: the bolt phosphating layer of the nuclear power equipment with reliable quality, uniformity, compactness and good corrosion resistance can be obtained.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a flow chart of a nuclear power plant bolt phosphating method according to a first embodiment of the invention;
FIG. 2 is a flow chart of a nuclear power plant bolt phosphating method according to a second embodiment of the invention.
Detailed Description
In order to solve the problems that the bolts in the prior art adopt high-temperature manganese series phosphating, the film is heavy and the phosphating difficulty is large, the specific idea of the invention is as follows: the method for phosphorizing the bolt of the nuclear power equipment comprises the following steps: s1, preprocessing the equipment bolt: firstly, soaking a bolt in deoiling liquid for deoiling treatment, washing the bolt at normal temperature after deoiling, washing the bolt with hydrochloric acid after washing, washing the bolt with water again after washing, and then performing surface conditioning; s2, soaking the pretreated bolt in a phosphating solution for a first preset time to carry out pre-phosphating; s3, reprocessing the pre-phosphorized bolt: washing the bolt with water again, washing with hydrochloric acid after washing with water, washing with water again after washing with acid, and then performing surface conditioning; and S4, soaking the retreated bolt in the phosphating solution again for a second preset time to perform phosphating. The method and the phosphating solution for phosphating the bolts of the nuclear power equipment can obtain the phosphating layers of the bolts of the nuclear power equipment, which are reliable in quality, uniform and compact and good in corrosion resistance.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Example one
As shown in fig. 1, a method for phosphorizing a bolt of a nuclear power plant in a first embodiment of the present invention includes the following steps:
s1, preprocessing the equipment bolt: firstly, soaking a bolt in deoiling liquid for deoiling treatment, washing the bolt at normal temperature after deoiling, washing the bolt with hydrochloric acid after washing, washing the bolt with water again after washing, and then performing surface conditioning;
s2, soaking the pretreated bolt in a phosphating solution for a first preset time to carry out pre-phosphating;
s3, reprocessing the pre-phosphorized bolt: washing the bolt with water again, washing with hydrochloric acid after washing with water, washing with water again after washing with acid, and then performing surface conditioning;
and S4, soaking the retreated bolt in the phosphating solution again for a second preset time to perform phosphating.
Example two
As shown in fig. 2, the method for phosphorizing the bolt of the nuclear power plant in the second embodiment of the invention further includes the following steps:
s5, post-processing the phosphated bolt: washing the bolt with water again, passivating the bolt with a passivating agent after washing with water, washing the bolt with water again after passivating, and drying the bolt to soak oil;
and S6, carrying out quality inspection on the phosphated bolt.
Specifically, in step S2 and step S4, the same phosphating solution is used for pre-phosphating and phosphating, and the phosphating solution comprises: the additive comprises 35g/L of Marshall salt, 20g/L of manganese nitrate and 3-5g/L of accelerator;
wherein the accelerator is selected from one or more of nitrite, nitrate or chlorate.
Specifically, the total acidity of the phosphating solution is 30-40 points, the acidity of free acid is 3-4 points, and the temperature of the pre-phosphating in the step S2 and the temperature of the phosphating process in the step S4 are both 80-90 ℃.
In the present example, the prephosphorization and the phosphating processes differ in terms of time duration, the first predetermined time duration of the prephosphorization process being 10 to 15 minutes and the second predetermined time duration of the phosphating process being 20 to 25 minutes.
Specifically, the step S1 specifically includes: soaking the bolt in deoiling liquid for deoiling treatment, wherein the deoiling liquid has the temperature of 80-90 ℃ and the deoiling time of 25-30 minutes, and the deoiling liquid comprises the following components: NaOH with a concentration of 30g/l, Na3PO4 with a concentration of 30g/l and Na2CO3 with a concentration of 40 g/l; washing the deoiled bolt with water at normal temperature; pickling the washed bolt with 15% HCl at normal temperature for 12-20 min; washing the bolt after acid washing again at normal temperature; and (4) performing surface adjustment on the bolt subjected to water cleaning again by adopting a surface adjusting liquid, wherein the PH control target of the surface adjusting liquid is 8, and the surface adjusting time is 1 minute.
Specifically, the step S3 specifically includes: washing the bolt with water at normal temperature; pickling the washed bolt with 15% HCl at normal temperature for 12-20 min; and (4) performing surface adjustment on the bolt subjected to water cleaning again by adopting a surface adjusting liquid, wherein the PH control target of the surface adjusting liquid is 8, and the surface adjusting time is 1 minute.
In this embodiment, step S5 specifically includes: washing the bolt with water at normal temperature; after washing, passivating by using a passivating agent with the concentration of 40g/L2Cr2O7The solution is passivated for 2 minutes at 60-70 ℃. After passivation, washing the bolt with water again; the bolts were dried and immersed in engine oil for 4 minutes at 110-.
Specifically, the quality check in step S6 specifically includes: after drying the phosphated bolt, carrying out appearance inspection under the brightness of not less than 500 lux, wherein the surface is smooth and complete, the phosphated layer has uniform color, the color is gray, dark gray and black gray, the surface has no corrosive and foreign matter visual inspection, the crystal is compact, the bolt has certain luster, and has no rust spot, stripe, metal bright spot and the like; and then carrying out an anti-corrosion test on the bolt, dripping a drop of liquid on the phosphate coating, observing the time from blue, light green, yellow to light red to detect whether the anti-corrosion performance of the bolt phosphate coating is qualified, wherein the test result takes more than 3 minutes as a qualification criterion, and then detecting whether the thickness of the phosphate coating is qualified, and the thickness is 5-10 mu m.
The main components of the dropping liquid are shown in the following table:
the main ingredients of the dropping liquid
Figure BDA0001510209680000061
EXAMPLE III
The third embodiment of the invention provides a phosphating solution for pre-phosphating and phosphating bolts of nuclear power equipment, which comprises the following steps: the additive comprises 35g/L of Marshall salt, 20g/L of manganese nitrate and 3-5g/L of accelerator; wherein the accelerator is selected from one or more of nitrite, nitrate or chlorate.
In this example, the total acidity of the phosphating solution was 30 to 40 points and the acidity of the free acid of the phosphating solution was 3 to 4 points.
To sum up, the scheme of the application has the following beneficial technical effects at least compared with the prior art: the bolt phosphating layer of the nuclear power equipment with reliable quality, uniformity, compactness and good corrosion resistance can be obtained.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (11)

1. A method for phosphorizing a bolt of nuclear power equipment is characterized by comprising the following steps:
s1, preprocessing the equipment bolt: firstly, soaking a bolt in deoiling liquid for deoiling treatment, washing the bolt at normal temperature after deoiling, washing the bolt with hydrochloric acid after washing, washing the bolt with water again after washing, and then performing surface conditioning;
s2, soaking the pretreated bolt in a phosphating solution for a first preset time to carry out pre-phosphating;
s3, reprocessing the pre-phosphorized bolt: washing the bolt with water again, washing with hydrochloric acid after washing with water, washing with water again after washing with acid, and then performing surface conditioning;
s4, soaking the retreated bolt in the phosphating solution again for a second preset time to carry out phosphating;
s5, post-processing the phosphated bolt: washing the bolt with water again, passivating the bolt with a passivating agent after washing with water, washing the bolt with water again after passivating, and drying the bolt to soak oil;
s6, carrying out quality inspection on the phosphated bolt;
the step S6 specifically includes: drying the phosphated bolt, performing appearance inspection under the brightness of not less than 500 lux, performing corrosion resistance test on the bolt to detect whether the corrosion resistance of the phosphated layer of the bolt is qualified or not, taking the test result of more than 3 minutes as a qualification criterion, and then detecting whether the thickness of the phosphated layer is qualified or not, wherein the thickness is 5-10 mu m.
2. The method for phosphating bolts of nuclear power equipment according to claim 1, wherein in the step S2 and the step S4, the same phosphating solution is adopted for pre-phosphating and phosphating, and the phosphating solution comprises: the additive comprises 35g/L of Marshall salt, 20g/L of manganese nitrate and 3-5g/L of accelerator;
wherein the accelerator is selected from one or more of nitrite, nitrate or chlorate.
3. The method for phosphating bolts of nuclear power equipment according to claim 1, wherein the phosphating solution has total acidity of 30-40 points, free acid acidity of 3-4 points, and both the pre-phosphating in step S2 and the phosphating process in step S4 have temperatures of 80-90 ℃.
4. The method of claim 1, wherein the first predetermined period of time is 10-15 minutes.
5. The method of claim 1, wherein the second predetermined period of time is 20-25 minutes.
6. The method for phosphorizing the bolt of the nuclear power equipment as recited in claim 1, wherein the step S1 specifically comprises:
soaking the bolt in deoiling liquid for deoiling treatment, wherein the deoiling liquid has the temperature of 80-90 ℃ and the deoiling time of 25-30 minutes, and the deoiling liquid comprises the following components: NaOH at a concentration of 30g/l, Na at a concentration of 30g/l3PO4And Na in a concentration of 40g/l2CO3；
Washing the deoiled bolt with water at normal temperature;
pickling the washed bolt with 15% HCl at normal temperature for 12-20 min;
washing the bolt after acid washing again at normal temperature;
and (4) performing surface adjustment on the bolt subjected to water cleaning again by adopting a surface adjusting liquid, wherein the PH control target of the surface adjusting liquid is 8, and the surface adjusting time is 1 minute.
7. The method for phosphorizing the bolt of the nuclear power equipment as recited in claim 1, wherein the step S3 specifically comprises:
washing the bolt with water at normal temperature;
pickling the washed bolt with 15% HCl at normal temperature for 12-20 min;
and (4) performing surface adjustment on the bolt subjected to water cleaning again by adopting a surface adjusting liquid, wherein the PH control target of the surface adjusting liquid is 8, and the surface adjusting time is 1 minute.
8. The method for phosphorizing the bolt of the nuclear power equipment as recited in claim 1, wherein the step S5 specifically comprises:
washing the bolt with water at normal temperature;
after washing, passivating by using a passivating agent with the concentration of 40g/L2Cr2O7Passivating the solution for 2 minutes at the passivation temperature of 60-70 ℃;
after passivation, washing the bolt with water again;
the bolts were dried and immersed in engine oil for 4 minutes at 110-.
9. A phosphating solution for carrying out the phosphating step according to any one of claims 1 to 8 for the pre-phosphating and phosphating of bolts for nuclear power plants, characterized in that it comprises: the additive comprises 35g/L of Marshall salt, 20g/L of manganese nitrate and 3-5g/L of accelerator;
wherein the accelerator is selected from one or more of nitrite, nitrate or chlorate.
10. The phosphating solution of claim 9, wherein the phosphating solution has a total acidity of 30-40 points.
11. The phosphating solution of claim 9, wherein the acidity of the free acid of the phosphating solution is 3-4 points.
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JP2011001626A (en) * 2009-06-18 2011-01-06 Nippon Parkerizing Co Ltd Method of treating surface of metal structure at low agitation speed
CN102534591B (en) * 2012-01-05 2013-12-18 安徽启明表面技术有限公司 Thick film phosphating method
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