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FR2601698A1 - Phosphating bath and process - Google Patents

Phosphating bath and process Download PDF

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Publication number
FR2601698A1
FR2601698A1 FR8610586A FR8610586A FR2601698A1 FR 2601698 A1 FR2601698 A1 FR 2601698A1 FR 8610586 A FR8610586 A FR 8610586A FR 8610586 A FR8610586 A FR 8610586A FR 2601698 A1 FR2601698 A1 FR 2601698A1
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FR
France
Prior art keywords
mixture
water
bath
sulphate
liters
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
FR8610586A
Other languages
French (fr)
Other versions
FR2601698B3 (en
Inventor
Rene Coillet-Matillon
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SOLYPRO NOUVELLE EXPLOIT
Original Assignee
SOLYPRO NOUVELLE EXPLOIT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SOLYPRO NOUVELLE EXPLOIT filed Critical SOLYPRO NOUVELLE EXPLOIT
Priority to FR8610586A priority Critical patent/FR2601698B3/en
Publication of FR2601698A1 publication Critical patent/FR2601698A1/en
Application granted granted Critical
Publication of FR2601698B3 publication Critical patent/FR2601698B3/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/07Chemical 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
    • C23C22/08Orthophosphates
    • C23C22/18Orthophosphates containing manganese cations
    • C23C22/188Orthophosphates containing manganese cations containing also magnesium cations

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

A new phosphating bath and process against rust and corrosion of metal articles, iron, cast iron, steel. The bath consists of a primary mixture A containing: 10 to 20 l of 75% phosphoric acid, 5 to 15 l of water, 150 to 200 g of iron powder and of a complementary mixture B containing: 5 to 6 kg of manganese, 5 to 6 kg of nickel sulphate, 3 to 4 kg of zinc sulphate, 2 to 3 kg of cobalt sulphate and 30 litres of water. This bath results from the addition of 26 l of the mixture A and 1/2 l of the complementary mixture B and is made up to 30 l with water. The process consists in immersing the articles in the phosphating bath at a temperature of 95 to 98 DEG C. The immersion period varies from 10 to 30 minutes depending on the chosen treatment, light or thicker, the latter solution having to give a more effective protection against rust. The articles are then withdrawn from the bath and are dried with a blower or in an oven.

Description

La présente invention concerne un nouveau bain et procédé de PHOSPHATATION contre la rouille et la corrosion des pièces métalliques, fer, fonte ou acier.The present invention relates to a new bath and PHOSPHATION process against rust and corrosion of metal parts, iron, cast iron or steel.

Notre invention est une méthode très efficace contre la rouille et de plus, constitue une base d'accrochage exceptionnelle pour peinture, teinture, bisulfure de molybdène MOS/2.Our invention is a very effective method against rust and moreover, constitutes an exceptional bonding base for painting, dyeing, molybdenum disulphide MOS / 2.

C'est à la suite de plusieurs années de recherches que le procédé a été mis au point, pour obtenir un résultat tout à fait satisfaisant pour son efficacité contre la rouille, et son aspect visuel, finition coloration noire - De plus cette méthode est très économique.It is after several years of research that the process was developed, to obtain a completely satisfactory result for its effectiveness against rust, and its visual appearance, finish black coloring - In addition this method is very economic.

Les pièces métalliques sont 1") Dégraissées aux vapeurs de TRICHLORETHANE commercialisé sous le nom
de SOLVETHENE (ou tout autre solvant convenant au nettoyage des pièces) 20) Sans autre opération, les pièces ainsi préparées peuvent subir le
traitement phosphatation
Le traitement consiste à Immerger les pièces dans le bain de phosphatation a mne température de 95 a C. Le temps dtimmersion varie de 10 à 20 minutes selon le traitement choisi, léger ou plus épais, cette dernière solution devant donner une protection plus efficace contre la rouille.
The metal parts are 1 ") Degreased with TRICHLORETHANE vapors marketed under the name
SOLVETHENE (or any other solvent suitable for cleaning the parts) 20) Without any other operation, the parts thus prepared can undergo the
phosphating treatment
The treatment consists of immersing the pieces in the phosphating bath at a temperature of 95 to C. The immersion time varies from 10 to 20 minutes depending on the treatment chosen, light or thicker, the latter solution having to give more effective protection against rust.

Les pièces sont ensuite retirées du bain, puis séchées à la soufflette ou en étuve,
L'opération de phosphatation est terminée.
The pieces are then removed from the bath, then dried in a blow gun or in an oven,
The phosphating operation is finished.

Les pièces ainsi traitées pourront recevoir un revetement de peinture, teinture, vernis, huile ou tout autres produits.The parts thus treated may receive a coating of paint, stain, varnish, oil or any other product.

Cette méthode est particulièrement souhaitable et recommandée pour ses qualités de base d'accrochage, notamment pour le bisulfure de molybdène
Elle n'écaille pas.
This method is particularly desirable and recommended for its basic bonding qualities, in particular for molybdenum disulphide
It does not flake.

Notre méthode très simple dans sa conception est d'un prix de revient nettement inférieur à tous les autres produits actuels.Our very simple method in its conception is of a cost price clearly lower than all the other current products.

Ces produits étant tous d'importation ou fabriqués sous licence (frais de transports, problèmes de délais de livraison, risque de grèves,
règlements par virements inter-bancaires ou comptants).
These products are all imported or manufactured under license (transport costs, delivery time problems, risk of strikes,
payments by inter-bank or cash transfers).

L'équipement pour l'utilisation de notre procédé est très simple et intéressant car ne necessite qu'une cuve de dégraissage et une cuve de phosphatation pour toute la réalisation du traitement.The equipment for the use of our process is very simple and interesting because it only requires a degreasing tank and a phosphating tank for the whole realization of the treatment.

L'entretien est minium
L'investissement est réalisé pour de très nombreuses années Le procédé est tout a fait inoffensif, et ne peut nuire a la santé des
personnes qui l'utilisent Ne demande pas mon personnel qualifié Il n'y a aucun risque de pollution, le bain n'étant jamais rejeté Il n'a aucune influence sur les propriétés physiques des métaux traités Le revêtement est de densité et d'épaisseur uniformes sur toute la
surface des pièces L'aspect des pièces est respecté.La surépaisseur de la couche est de
3 å su microns 2/3 å l'extérieur du métal, 1/3 à l'intérieur, fournissant
ainsi tne parfaite base d'accrochage Elle convient a tous les métaux, pièces msinéesss ressorts, aciers à haute
tension, les objets matricés, fondus, estampés, soit tous les aciers, fer,
fonte Alors que nombreuses autres méthodes exigent un rinçage des pièces après
traitement, cette opération se révèle totalement inutile avec notre pro
cédé de phosphatation Le prix ae revient du traitement est peu onéreux (fabriqué en France)
La cuve de phosphatation est en acier, de formes rectangulaires de dimensions permettant le meilleur usage, chauffée par l'électricité, le gaz ou la vapeur, calorifugée et toujours fermée d'un couvercle, afin d'éviter l'évaporation, la solution de traitement étant chauffée 24/24 h à la température constante de 95/98 C, contrôlée par thermostats. L'eau est fournie automatiquement ou manuellement, l'addition de produit de phosphatation est effectuée fréquemment, système à la convenance, et par petites quantités.
Maintenance is minimal
The investment is made for many years. The process is completely harmless, and cannot harm the health of
people who use it Do not ask my qualified personnel There is no risk of pollution, the bath is never rejected It has no influence on the physical properties of the treated metals The coating is of density and thickness uniforms all over
surface of the parts The appearance of the parts is respected. The thickness of the layer is
3 å on microns 2/3 outside the metal, 1/3 inside, providing
thus a perfect attachment base It is suitable for all metals, mechanical parts, springs, high steels
tension, stamped, melted, stamped objects, i.e. all steels, iron,
While many other methods require parts to be flushed after
treatment, this operation is completely useless with our pro
ceded with phosphating The cost price of the treatment is inexpensive (made in France)
The phosphating tank is made of steel, rectangular shapes of dimensions allowing the best use, heated by electricity, gas or steam, insulated and always closed with a lid, in order to avoid evaporation, the solution of treatment being heated 24/24 h at a constant temperature of 95/98 C, controlled by thermostats. The water is supplied automatically or manually, the addition of phosphate product is carried out frequently, system at convenience, and in small quantities.

Le bain de phosphatation se régénère avec l'eau courante additionnée de produit, le niveau est contrôlé et rectifié régulièrement.The phosphating bath is regenerated with running water added with product, the level is checked and adjusted regularly.

Le contrôle du bain consiste à maintenir l'équilibre du point d'acidité par l'addition du produit de phosphatation après un simple titrage du degré d'acidité, qui est réalisé en prélevant un échantillon dans la cuve de phosphatation à l'aide d'une pipette, et d'effectuer un contrôle visuel dans une éprouvette avec une solution indicatrice de titrage.Bath control consists in maintaining the equilibrium of the acidity point by adding the phosphating product after a simple titration of the degree of acidity, which is carried out by taking a sample from the phosphating tank using '' a pipette, and carry out a visual check in a test tube with a titration indicator solution.

Cette opération d'une grande simplicité et fiabilité peut-être réalisée par une personne non qualifiée.This operation of great simplicity and reliability can be carried out by an unqualified person.

La cuve de phosphatation ne nécessite aucun entretien excessif, il suffit de nettoyer les dépôts au fond de la cuve, et la décalaminer environ tous les cinq ans.The phosphating tank does not require any excessive maintenance, it suffices to clean the deposits at the bottom of the tank, and to decarbonize it approximately every five years.

Notre procédé est d'une utilisation très simple, comportant 3 phases
Dégraissage des pièces
. TraItement dans le bain de phosphatation
. Séchage
Les anciennes formules de phosphatation à base de zinc fixaient très mal le bisulfure de molybdène, d'où écaillage,qui rendait les pièces impropres à l'usage demandé.
Our process is very simple to use, comprising 3 phases
Degreasing of parts
. Treatment in the phosphating bath
. Drying
The old zinc-based phosphating formulas did not fix the molybdenum disulphide very well, hence flaking, which made the parts unsuitable for the required use.

Cette nouvelle formule à la particularité de fixer ce molybdène sans risque d'écaillage,
Le gros avantage de notre invention est aussi son coût, nettement inférieur aux prix de revient des antres procédés.
This new formula has the particularity of fixing this molybdenum without risk of chipping,
The big advantage of our invention is also its cost, much lower than the cost price of other processes.

A TITRE D'EXEMPLE NON LIMITATIF, NOUS ALLONS DONNER IA FORMULE SUIVANTE 1 ) On réalise le mélange primaire A
entre J0 et 20 1 d'acide phosphorique à 75 %
entre 5 et 15 1 d'eau
entre 150 et 250 g de poudre de fer
On laisse dissoudre 3 à 4 jours en remuant 20) On réalise le mélange complémentaire B
5 à 6 KG de manganèse
5 à 6 KG de sulfate de nickel
3 à 4 KG de sulfate de zinc
2 à 3 KG de sulfate de magnésie
1 à 2 KG de sulfate de cobalt
30 litres d'eau
On laisse sous agitation intermittente (toutes les 2 à 3 heures)
pendant 2 à 3 jours.
BY way of nonlimiting example, we will give the following formula 1) the primary mixture A is produced.
between D0 and 20 1 of 75% phosphoric acid
between 5 and 15 1 of water
between 150 and 250 g of iron powder
It is left to dissolve for 3 to 4 days, stirring 20) The complementary mixture B is produced
5 to 6 KG of manganese
5 to 6 kg of nickel sulfate
3 to 4 kg of zinc sulfate
2 to 3 kg of magnesia sulfate
1 to 2 kg of cobalt sulfate
30 liters of water
It is left with intermittent stirring (every 2 to 3 hours)
for 2 to 3 days.

30) On mélange 26 litres du mélange primaire A et 1/2 litre du mélange
complémentaire B, et on complète à 30 litres avec de l'eau.
30) 26 liters of primary mixture A and 1/2 liter of the mixture are mixed
complementary B, and make up to 30 liters with water.

'A TITRE D'EXEMPLE, NOUS ALLONS DONNER LA FORMULE SUIVANTE : 1Q) On réalise le mélange primaire A
16 1 d'acide phosphorique à 75 % 10 1 d'eau
200 g de poudre de fer
On laisse dissoudre 3 à 4 jours en remuant 20) On réalise le mélange complementaire B
5,500 KG de manganèse
5?300 KS de sulfate de nickel
3,750 KG de sulfate de zinc
2,850 KG de sulfate de magnésie
1,525 Kg de sulfate de cobalt
30 litres d'eau
On laisse sous agitation intermittente (toutes les 2 à 3 heures)
pendant 2 à 3 jours 33 On mélange 26 litres du mélange A et 1/2 litre du mélange complé-
inventaire B, et on complète à 30 litres avec de l'eau.
'AS AN EXAMPLE, WE WILL GIVE THE FOLLOWING FORMULA: 1Q) The primary mixture A is produced
16 1 of 75% phosphoric acid 10 1 of water
200 g iron powder
Leave to dissolve for 3 to 4 days, stirring 20) Complementary mixing B is carried out
5,500 KG of manganese
5? 300 KS of nickel sulphate
3,750 KG of zinc sulphate
2,850 kg of magnesia sulfate
1.525 Kg of cobalt sulfate
30 liters of water
It is left with intermittent stirring (every 2 to 3 hours)
for 2 to 3 days 33 26 liters of mixture A and 1/2 liter of the complete mixture are mixed
inventory B, and make up to 30 liters with water.

Claims (2)

RETENDICATIONS A Bain de phosphatation caractérisé en ce qu'il est constitué d'un mélange primaire A, contenant une solution aqueuse d'acide phospho rique, de poudre de fer, et d'un mélange complémentaire B, compor tant du manganèse, du sulfate de nickel, du sulfate de zinc, du sul fate de magnésie, du sulfate de cobalt, dissouts dans l'eau. t Bain selon la revendication 1, caractérisé en ce que le mélange primaire A comporte entre 10 et 20 1 d'acide phosphorique à 75 i, entre 5 et 15 1 d'eau, entre 150 et 250 g de poudre de fer, et en ce que le mélange complémentaire B comporte entre 5 et 6 KG de man ganèse, entre 5 et 6 KG de sulfate de nickel, entre 3 et 4 KG de sulfate de zinc, entre 2 et 3 KG de sulfate de magnésie, entre 1 etCLAIMS A Phosphating bath characterized in that it consists of a primary mixture A, containing an aqueous solution of phosphoric acid, iron powder, and a complementary mixture B, comprising manganese, sulphate nickel, zinc sulfate, magnesium sulfate, cobalt sulfate, dissolved in water. t Bath according to claim 1, characterized in that the primary mixture A comprises between 10 and 20 1 of phosphoric acid at 75 i, between 5 and 15 1 of water, between 150 and 250 g of iron powder, and in what the complementary mixture B comprises between 5 and 6 kg of manganese, between 5 and 6 kg of nickel sulphate, between 3 and 4 kg of zinc sulphate, between 2 and 3 kg of magnesia sulphate, between 1 and 2 KG de sulfate de cobalt, et 30 litres d'eau, et en ce que l'on 2 kg of cobalt sulfate, and 30 liters of water, and in that one additionne 26 litres du mélange primaire A, à 1/2 litre du mélange add 26 liters of primary mixture A, to 1/2 liter of the mixture complémentaire B, auquel on ajoute 30 litres d'eau. complementary B, to which 30 liters of water are added. 2 Bain selon la revendication 2, caractérisé en ce que le mélange pri 2 bath according to claim 2, characterized in that the mixture pri maire comporte 16 1 d'acide phosphorique à 75 %, 10 1 d'eau, 200 g mayor has 16 1 of 75% phosphoric acid, 10 1 of water, 200 g de poudre de fer, et en ce que le mélange complémentaire comporte of iron powder, and in that the complementary mixture comprises 5,500 KG de manganèse, 5,300 KG de sulfate de nickel, 3,750 KG de 5,500 KG of manganese, 5,300 KG of nickel sulphate, 3,750 KG of sulfate de zinc, 2,850 KG de sulfate de magnésie, 1,525 KG de sulfate zinc sulfate, 2,850 KG of magnesia sulfate, 1,525 KG of sulfate de cobalt, 30 litres d'eau, et en ce que l'on additionne 26 litres du of cobalt, 30 liters of water, and adding 26 liters of the mélange primaire A, à 1/2 litre du mélange complémentaire B, auquel primary mixture A, to 1/2 liter of the complementary mixture B, to which on ajoute 30 litres d'eau. 30 liters of water are added. 4 Procédé de phosphatation caractérisé en ce qu'il consiste à dégraisser 4 Phosphating process characterized in that it consists in degreasing les pièces, à les traiter dans un bain de phosphatation selon l'une des the parts, to treat them in a phosphating bath according to one of the revendications en 1 à 3, et à les sécher. claims 1 to 3, and to dry them. S Procédé selon la revendication 4, caractérisé en ce que les pièces sont S Method according to claim 4, characterized in that the parts are imsergees dans ie bain de phosphatation à une température de 95 à 98" C immersed in the phosphating bath at a temperature of 95 to 98 "C pendant un temps Variant de 10 à 20 minutes.  for a time varying from 10 to 20 minutes.
FR8610586A 1986-07-17 1986-07-17 BATH AND PHOSPHATATION PROCESS Expired FR2601698B3 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
FR8610586A FR2601698B3 (en) 1986-07-17 1986-07-17 BATH AND PHOSPHATATION PROCESS

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR8610586A FR2601698B3 (en) 1986-07-17 1986-07-17 BATH AND PHOSPHATATION PROCESS

Publications (2)

Publication Number Publication Date
FR2601698A1 true FR2601698A1 (en) 1988-01-22
FR2601698B3 FR2601698B3 (en) 1988-10-21

Family

ID=9337602

Family Applications (1)

Application Number Title Priority Date Filing Date
FR8610586A Expired FR2601698B3 (en) 1986-07-17 1986-07-17 BATH AND PHOSPHATATION PROCESS

Country Status (1)

Country Link
FR (1) FR2601698B3 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0711849A1 (en) * 1994-11-11 1996-05-15 Metallgesellschaft Aktiengesellschaft Process for applying phosphate coatings
WO1996017977A1 (en) * 1994-12-09 1996-06-13 Metallgesellschaft Aktiengesellschaft Method of applying phosphate coatings to metal surfaces

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0711849A1 (en) * 1994-11-11 1996-05-15 Metallgesellschaft Aktiengesellschaft Process for applying phosphate coatings
WO1996017977A1 (en) * 1994-12-09 1996-06-13 Metallgesellschaft Aktiengesellschaft Method of applying phosphate coatings to metal surfaces
US5904786A (en) * 1994-12-09 1999-05-18 Metallgesellschaft Aktiengesellschaft Method of applying phosphate coatings to metal surfaces

Also Published As

Publication number Publication date
FR2601698B3 (en) 1988-10-21

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