CN101543943B

CN101543943B - Leadless rosin core low-halogen no-clean scaling powder and method for preparing same

Info

Publication number: CN101543943B
Application number: CN200910094413XA
Authority: CN
Inventors: 秦俊虎; 刘宝权; 李树祥; 吕金梅
Original assignee: YUNNAN TIN MATERIAL CO Ltd
Current assignee: Yunnan Tin New Material Co ltd
Priority date: 2009-04-29
Filing date: 2009-04-29
Publication date: 2012-07-11
Anticipated expiration: 2029-04-29
Also published as: CN101543943A

Abstract

The invention provides a formulation of leadless rosin core low-halogen no-clean scaling powder and a method for preparing the same. The formulation comprises the following components by weight percentage: 4.0 to 7.0 percent of organic solvent, 1.0 to 2.0 percent of hydroxyl organic acid in an active agent, 0.5 to 0.8 percent of halogenated organic acid in the active agent, 0.2 to 0.6 percent of surfactant, and the balance of common hydrogenated rosin. The scaling powder prepared by the method has the advantages of low cost, good weldability and low corrosivity, which not only can save the cost for solder manufacturers, but also better solves the existing contradictions between poor weld and weldability and corrosivity.

Description

Leadless rosin core low-halogen no-clean scaling powder and preparation method thereof

One, technical field

The present invention relates to prescription of a kind of leadless rosin core low-halogen no-clean scaling powder and preparation method thereof, as lead-free soldering wire help the wlding material, belong to technical field of welding materials.

Two, background technology

Solder stick is mainly used in welding, repair welding and the maintenance of instrument, instrument, various household electrical appliance etc., but along with the enhancing of human environmental consciousness, unleaded welding is imperative, and lead-free soldering wire is also used and given birth to.Meanwhile, the quality of welding quality not only depends on the alloy material of solder stick, more depends on the performance of its core with scaling powder, thereby the no lead for retractable pencil of research just seems particularly important with scaling powder.

China is in from having plumbous to the unleaded excessive and starting stage; Though it is of a great variety with scaling powder not have lead for retractable pencil; But also there is certain problem, mainly shows lower, be applied to exist in the solder stick shortcomings such as the solder joint outward appearance is coarse, the rate of spread is little, angle of wetting is big with the flux activity of common Foral preparation; And it is good with the flux activity of the Foral of higher level preparation; But cost is very high, in addition, has also that active agent content is high, the high big and activating agent of corrosivity that causes of content of halogen disperses the inhomogeneous problem such as spatter that causes in rosin.

Prescription according to disclosing the related patent U.S. Patent No. document can be known: at present, the method that overcomes the above problems is: the low-cost film forming agent that uses higher level is abandoned in (1), just uses the higher rosin of purity and acid number.Such as, the rosin that the patent that has is used is expensive high-level rosin such as water-white rosin, superfine Foral, perhydrogenated rosin, KE-604; (2) abandon low-corrosiveness and increase organic acid content and interpolation halo amine salt in the scaling powder, the i.e. hydrochloride of amine or bromate.Such as, it is more than 10% that the patent that has is used active agent content; The patent that also has is with the hydrochloride or the bromate of amine.

Three, summary of the invention

The objective of the invention is to overcome the weld defect of existing solder stick, a kind of leadless rosin core low-halogen no-clean scaling powder and preparation method thereof is provided, its low cost, high activity, low burn into good welding performance.

In order to reach above the object of the invention, the present invention takes following technical scheme:

Scaling powder is formed and the quality percentage composition is: organic solvent 4.0%～7.0%, hydroxy organic acid activating agent 1.0%～2.0%, halogen organic acid activating agent 0.5%～0.8%, surfactant 0.2%～0.6%, surplus are common Foral; The physical and chemical index of described common Foral is inferior to the index of GB GB/T14020-92, i.e. acid number≤160mgKOH/g, unsaponifiable matter>=8%, oxygen uptake>=0.2%, abietic acid>=2.5%.

Further technical scheme of the present invention is:

Described hydroxy organic acid activating agent adopts in tartaric acid, ten dihydroxystearic acids, itaconic acid or the malic acid any two kinds; Any mixes the hydroxy organic acid activating agent with the halogen organic acid activating agent mutually in halogen organic acid activating agent employing dibromosuccinic acid, 2-chloro-4-bromobenzoic acid, the 2-fluoro-4-bromobenzoic acid.

Described organic solvent is any two kinds of mixtures in ethanol, isopropyl alcohol, glycerine, the dibutyl ethylene glycol ether.

Described surfactant is the nonionic glycerol caprylate, cetyl stearic, lauroyl monoethanolamine, any in glycerin polyoxyethylene (7), (26) ether.

The preparation scheme of above-mentioned leadless rosin core low-halogen no-clean scaling powder is following:

1) the common Foral of fusion in a reactor, temperature is 130 ℃～150 ℃;

2) in the another one reactor, prepare active liquid, the preparation method stirred 5～10 minutes for according to the above ratio solvent being added in the reactor; Be warmed up to 50 ℃～80 ℃ then; Add activating agent and surfactant more successively, continue to stir 15～20 minutes, it is mixed;

3) active liquid is slowly added in the molten rosin, cooling promptly gets the leadless rosin core no-clean scaling powder.

In above-mentioned preparation process, active liquid should remain on 90 ℃～120 ℃ with temperature after adding in the molten rosin, stirs 20～40 minutes, cools off again.

Innovative point of the present invention is:

(1) film forming matter is common Foral, does not use expensive water-white rosin, superfine Foral, perhydrogenated rosin, KE-604 etc., to reduce entreprise cost, realizes the low cost strategy of enterprise.

(2) select the activating agent of different activation temperature gradients composite, further be: select to have hydroxy organic acid activating agent composite of different activation temperature gradients, this can make the low temperature active agent when welding temperature is low, have activity on the one hand; And it can also induce, excite the high temperature active agent; Make activating agent in the whole temperature range of welding, all have activity, thus improve scaling powder help the weldering effect, on the other hand; Through using hydroxyl organic acid can strengthen the organic acid activity; Thereby reduce the content of organic acid in scaling powder, further reduce corrosivity, reach the unification of strong activity and low-corrosiveness.

(3) halogenated acid of use covalent bond because the halogen in the halo amine salt is an ionic bond, goes out halogen open circuit potential plate thereby be easy to ionization; And can effectively prevent halogen ionization as the halogenated acid of covalent bond; In addition, halogen atom is an electron withdraw group, makes the hydroxyl in the organic acid that ionization take place more easily; Further improve flux activity, reach low halogen, highly active purpose.

(4) use little solvent lytic activity agent and surfactant, the method that joins rosin to active liquid then can make activating agent in rosin, be uniformly dispersed, and reduces spatter.

In a word; The present invention makes common Foral just can reach highly active effect through above innovation, thereby has reduced the cost of enterprise, meanwhile; Also reduced the use amount of activating agent; Better solved the weldability and the corrosivity contradiction of present existence, in addition, also reduced because of the inhomogeneous spatter phenomenon that produces of activating agent dispersion.

Four, specific embodiments

Embodiment 1

Concrete preparation method:

1) the common Foral of fusion in a reactor, temperature is 130 ℃～150 ℃.

2) in the another one reactor, prepare active liquid, the preparation method is in the solvent adding reactor by a certain percentage, stirs 5～10 minutes, is warmed up to 50 ℃～80 ℃ then, adds activating agent and surfactant successively, continues to stir 15～20 minutes.

3) active liquid is slowly added in the molten rosin, temperature remains on 90 ℃～120 ℃, stirs 20～40 minutes, and cooling promptly gets the leadless rosin core no-clean scaling powder.

Embodiment 2

The preparation method is identical with embodiment 1.

Embodiment 3

The preparation method is identical with embodiment 1.

Embodiment 4

The preparation method is identical with embodiment 1.

Through enforcement of the present invention; The leadless rosin core low-halogen no-clean scaling powder of preparing has not only reduced the cost of enterprise; And the purpose that has reached high activity, hanged down halogen; Well solved active and corrosive contradiction, in addition, also reduced because of the inhomogeneous spatter that produces of activating agent dispersion.

Claims

1. leadless rosin core low-halogen no-clean scaling powder, it is characterized in that: each material is formed according to following percentage by weight: organic solvent 4.0%～7.0%, hydroxy organic acid activating agent 1.0%～2.0%, halogen organic acid activating agent 0.5%～0.8%, surfactant 0.2%～0.6%, surplus are common Foral; And the index of common Foral is acid number≤160mgKOH/g, unsaponifiable matter>=8%, oxygen uptake>=0.2%, abietic acid>=2.5%.

2. leadless rosin core low-halogen no-clean scaling powder according to claim 1 is characterized in that: organic solvent is any two kinds of mixtures in ethanol, isopropyl alcohol, glycerine, the dibutyl ethylene glycol ether.

3. leadless rosin core low-halogen no-clean scaling powder according to claim 1; It is characterized in that: the hydroxy organic acid activating agent adopts in tartaric acid, ten dihydroxystearic acids, itaconic acid or the malic acid any two kinds; Any mixes the hydroxy organic acid activating agent with the halogen organic acid activating agent mutually in halogen organic acid activating agent employing dibromosuccinic acid, 2-chloro-4-bromobenzoic acid, the 2-fluoro-4-bromobenzoic acid.

4. leadless rosin core low-halogen no-clean scaling powder according to claim 1 is characterized in that: surfactant is the nonionic glycerol caprylate, cetyl stearic, lauroyl monoethanolamine, any in glycerin polyoxyethylene (7), (26) ether.

5. the preparation method of the described leadless rosin core low-halogen no-clean scaling powder of claim 1; It is characterized in that: in two reactors, prepare active liquid and the common Foral of fusion respectively, the preparation method of active liquid stirred 5～10 minutes in proportion organic solvent being added in the reactor; Be warmed up to 50 ℃～80 ℃ then; Add activating agent and surfactant more successively, continue to stir 15～20 minutes, it is mixed; In another reactor, at 130 ℃～150 ℃ common Forals of following fusion, active liquid is slowly added in the molten rosin, cooling promptly gets the leadless rosin core no-clean scaling powder again.

6. the preparation method of leadless rosin core low-halogen no-clean scaling powder according to claim 5 is characterized in that: after in the active liquid adding molten rosin, should temperature be remained on 90 ℃～120 ℃, stir 20～40 minutes.